CN110265191A - SrTiO3Polycrystalline circle substrate and preparation method thereof - Google Patents
SrTiO3Polycrystalline circle substrate and preparation method thereof Download PDFInfo
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- CN110265191A CN110265191A CN201910518122.2A CN201910518122A CN110265191A CN 110265191 A CN110265191 A CN 110265191A CN 201910518122 A CN201910518122 A CN 201910518122A CN 110265191 A CN110265191 A CN 110265191A
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- H01B12/00—Superconductive or hyperconductive conductors, cables, or transmission lines
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Abstract
The present invention relates to a kind of SrTiO3The preparation method of polycrystalline circle substrate comprising following steps: by a untreated SrTiO3Polycrystalline circle substrate is placed in a vacuum chamber, and the pressure of the vacuum chamber is lower than 10‑9Mbar, wherein the untreated SrTiO3Polycrystalline circle substrate includes the SrTiO that multiple coplanar splicings are arranged and crystal orientation is different3Single crystalline substrate, adjacent S rTiO3There is groove, and each SrTiO between single crystalline substrate3Single crystalline substrate surface is that non-atomic grade is smooth；And by the untreated SrTiO3Polycrystalline circle silicon is to 1050 DEG C or more, to the untreated SrTiO3Polycrystalline circle substrate annealing 10 minutes or more.The invention further relates to a kind of SrTiO prepared using the above method3Polycrystalline circle substrate comprising: the SrTiO that multiple coplanar splicings are arranged and crystal orientation is different3Single crystalline substrate, wherein adjacent S rTiO3Crystal boundary between single crystalline substrate heals completely, forms atomic level contact, and each SrTiO3Single crystalline substrate surface is atomically flating.
Description
Technical field
The present invention relates to superconductor technology field more particularly to SrTiO3Polycrystalline circle substrate and preparation method thereof.
Background technique
High-temperature superconductor is a kind of non-conventional superconductor that cannot be explained with traditional BCS theory.1986, Miller and shellfish
De-Nol that thatch has found copper oxygen compound high-temperature superconductor for the first time.2008, Japanese Scientists had found that iron-based high temp is super for the first time
Conductor.Since the superconducting transition temperature peak of iron-based high-temperature superconductive body changes far below the highest of copper oxide high temperature superconductor
Temperature, iron-based high-temperature superconductive body get more and more people's extensive concerning.
Referring to the Chinese patent application of Publication No. CN103184513A, open one kind is in SrTiO3Substrate surface growth
The method of FeSe high-temperature superconducting thin film, wherein by the SrTiO3It is super that substrate is placed in growth FeSe high temperature in ultra-high vacuum system
Before leading film, need to the SrTiO3Substrate carries out boiling processing, acid processing and air high temperature annealing respectively, to obtain
With atomically flating step and single TiO2The SrTiO of terminal surface3Substrate.
Referring to the Chinese patent application of Publication No. CN105679647A, it is open it is a kind of have atomically flating surface and
The SrTiO of FeSe high-temperature superconducting thin film can be grown3The preparation method of substrate, this method comprises: providing identical material at least
Two pre-processed substrates, each pre-processed substrate have an at least burnishing surface；By at least two pre-processed substrates layer
It folds setting and forms a laminate structure, wherein the burnishing surface of two adjacent pre-processed substrates is opposite and completely heavy
Folded setting；The laminate structure is placed on after being made annealing treatment in air in high temperature furnace, separates the laminate structure.
Wherein, pre-processed substrate includes boiling processing and acid processing.
However, above-mentioned processing SrTiO3In the method for substrate, to the SrTiO3Substrate carry out boiling processing, acid processing and
The high temperature anneal is carried out in air, is required to special treatment fluid and annealing device, and technique is cumbersome, higher cost.
Summary of the invention
The present invention provides a kind of SrTiO3The preparation method of polycrystalline circle substrate, this method are not necessarily to untreated SrTiO3Lining
Bottom carries out boiling processing, acid processing and carries out high-temperature heat treatment in air, can obtain having atomically flating surface
SrTiO3Substrate.
A kind of SrTiO3The preparation method of polycrystalline circle substrate comprising following steps: by a untreated SrTiO3Polycrystalline circle
Substrate is placed in a vacuum chamber, and the pressure of the vacuum chamber is lower than 10-9Mbar, wherein the untreated SrTiO3Polycrystalline circle substrate
Including multiple coplanar splicing settings and the different SrTiO of crystal orientation3Single crystalline substrate, adjacent S rTiO3There is groove between single crystalline substrate,
And each SrTiO3Single crystalline substrate surface is that non-atomic grade is smooth；And by the untreated SrTiO3Polycrystalline circle silicon is extremely
1050 DEG C or more, to the untreated SrTiO3Polycrystalline circle substrate annealing 10 minutes or more.
A kind of SrTiO prepared using the above method3Polycrystalline circle substrate comprising: multiple coplanar splicing settings and crystal orientation
Different SrTiO3Single crystalline substrate, wherein adjacent S rTiO3Crystal boundary between single crystalline substrate heals completely, forms atomic level contact,
And each SrTiO3Single crystalline substrate surface is atomically flating.
Compared to the prior art, SrTiO provided by the invention3The preparation method of polycrystalline circle substrate, without to untreated
SrTiO3Substrate carries out boiling processing, acid processing and carries out high-temperature heat treatment in air, can obtain flat with atom level
The SrTiO on whole surface3Substrate.Moreover, SrTiO provided by the invention3The preparation method of polycrystalline circle substrate is annealed by ultrahigh vacuum
Processing, can make adjacent S rTiO3Crystal boundary between single crystalline substrate heals completely forms atomic level contact.This method preparation
SrTiO3In polycrystalline circle substrate, adjacent S rTiO3Crystal boundary between single crystalline substrate heals completely forms atomic level contact.
Detailed description of the invention
Fig. 1 is processing SrTiO provided in an embodiment of the present invention3The method schematic diagram of substrate.
Fig. 2 is the SrTiO before annealing provided in an embodiment of the present invention and after annealing3The structural schematic diagram of twin boundary substrate.
Fig. 3 is the structural schematic diagram of the FeSe twin boundary superconductor provided in an embodiment of the present invention with groove and gap.
Fig. 4 is the structural schematic diagram provided in an embodiment of the present invention without groove and the FeSe twin boundary superconductor in gap.
Fig. 5 is the SrTiO with atomically flating surface prepared by the embodiment of the present invention 13The scanning-tunnelling of single crystalline substrate
Microscope (STM) photo.
Fig. 6 is the SrTiO of non-oxygenating processing prepared by the embodiment of the present invention 13Substrate growth FeSe high-temperature superconducting thin film
As a result scanning tunneling microscope photo.
Fig. 7 is the scanning tunneling microscope photo before FeSe high-temperature superconducting thin film annealing prepared by the embodiment of the present invention 2.
Fig. 8 is the scanning tunneling microscope photo after FeSe high-temperature superconducting thin film annealing prepared by the embodiment of the present invention 2.
Fig. 9 is the SrTiO for the unannealed processing that the embodiment of the present invention 3 provides3The atomic force microscope of twin boundary substrate
(AFM) photo.
Figure 10 is the SrTiO after the annealing that the embodiment of the present invention 3 provides3The scanning tunneling microscope of twin boundary substrate
Photo.
Figure 11 is that the scanning tunneling microscope before FeSe high-temperature superconducting thin film annealing prepared by the embodiment of the present invention 4 is shone
Piece.
Figure 12 is that the scanning tunneling microscope after FeSe high-temperature superconducting thin film annealing prepared by the embodiment of the present invention 4 is shone
Piece.
Figure 13 is the SrTiO after the annealing that the embodiment of the present invention 5 provides3The scanning tunneling microscope of twin boundary substrate
Photo.
Figure 14 is that the scanning tunneling microscope of the FeSe high-temperature superconducting thin film of 1UC thickness prepared by the embodiment of the present invention 6 is shone
Piece.
Figure 15 is that the scanning tunneling microscope of the FeSe high-temperature superconducting thin film of 10UC thickness prepared by the embodiment of the present invention 6 is shone
Piece.
Figure 16 is the SrTiO after the annealing that the embodiment of the present invention 7 provides3The scanning tunneling microscope of twin boundary substrate
Photo.
Figure 17 is the scanning tunneling microscope photo before FeSe high-temperature superconducting thin film annealing prepared by the embodiment of the present invention 8.
Figure 18 is the scanning tunneling microscope photo after FeSe high-temperature superconducting thin film annealing prepared by the embodiment of the present invention 8.
Figure 19 is the low-temperature scanning tunneling microscope of the grain boundaries of FeSe high-temperature superconducting thin film prepared by the embodiment of the present invention 8
Photo.
Figure 20 is that the FeSe single crystalline layer low temperature on the left of the crystal boundary of FeSe high-temperature superconducting thin film prepared by the embodiment of the present invention 8 is swept
Retouch tunnel microscope photo.
Figure 21 is that the FeSe single crystalline layer low temperature on the right side of the crystal boundary of FeSe high-temperature superconducting thin film prepared by the embodiment of the present invention 8 is swept
Retouch tunnel microscope photo.
Figure 22 is the scanning tunneling microscope photo before FeSe high-temperature superconducting thin film annealing prepared by the embodiment of the present invention 9.
Figure 23 is the scanning tunneling microscope photo after FeSe high-temperature superconducting thin film annealing prepared by the embodiment of the present invention 9.
Figure 24 is the SrTiO after the annealing that the embodiment of the present invention 10 provides3The scanning tunneling microscopic of twin boundary substrate
Mirror photo.
Figure 25 is the scanning tunneling microscope photo before FeSe high-temperature superconducting thin film annealing prepared by the embodiment of the present invention 11.
Figure 26 is the scanning tunneling microscope photo after FeSe high-temperature superconducting thin film annealing prepared by the embodiment of the present invention 11.
Figure 27 is the SrTiO after the annealing that the embodiment of the present invention 12 provides3The scanning tunneling microscopic of twin boundary substrate
Mirror photo.
Figure 28 is the scanning tunneling microscope photo before FeSe high-temperature superconducting thin film annealing prepared by the embodiment of the present invention 13.
Figure 29 is the scanning tunneling microscope photo after FeSe high-temperature superconducting thin film annealing prepared by the embodiment of the present invention 13.
Figure 30 is the SrTiO after the annealing that comparative example 1 of the present invention provides3The scanning tunneling microscope of single crystalline substrate is shone
Piece.
Figure 31 is the SrTiO after the annealing that comparative example 2 of the present invention provides3The scanning tunneling microscope of twin boundary substrate
Photo.
Figure 32 is the SrTiO after the annealing that comparative example 3 of the present invention provides3The atomic force microscope of twin boundary substrate is shone
Piece.
Figure 33 is the R-T test result of FeSe high-temperature superconducting thin film prepared by the embodiment of the present invention 6.
Figure 34 is the enlarged drawing of Figure 33 Blocked portion.
Figure 35 is the R-T test result of FeSe high-temperature superconducting thin film prepared by the embodiment of the present invention 8.
Figure 36 is the enlarged drawing of Figure 35 Blocked portion.
Figure 37 is the R-T test result that the embodiment of the present invention 13 prepares FeSe high-temperature superconducting thin film.
Main element symbol description
| FeSe superconductor | 10,10A |
| SrTiO3Substrate | 100 |
| Groove | 1002 |
| First electrode | 101 |
| Second electrode | 102 |
| Heating element | 103 |
| FeSe high-temperature superconducting thin film | 104 |
| Gap | 1042 |
| Vacuum chamber | 20 |
Specific embodiment
The present invention is described in further detail below in conjunction with the accompanying drawings and the specific embodiments.
In order to make it easy to understand, the present invention first introduces SrTiO provided in an embodiment of the present invention3The processing method of substrate, and
Using treated the SrTiO3The method of substrate growth FeSe superconductor.
Referring to Fig. 1, the embodiment of the present invention provides a kind of processing SrTiO3The method of substrate comprising following steps:
Step S10, by a SrTiO3Substrate 100 is placed in a vacuum chamber 20, and the pressure of the vacuum chamber 20 is lower than 10- 9Mbar, the SrTiO3100 surface of substrate is that non-atomic grade is smooth；And
Step S20, by the SrTiO3Substrate 100 is heated to 900 DEG C or more, to the SrTiO3Substrate 100 anneal 30 minutes with
On.
In the step S10, the SrTiO3Substrate 100 can be single crystalline substrate, or polycrystalline circle substrate.It is described
It includes a monocrystal that single crystalline substrate, which refers to the substrate only,.Referring to fig. 2, it includes multiple coplanar that the polycrystalline circle substrate, which refers to the substrate only,
The SrTiO that splicing is arranged and crystal orientation is different3Single crystalline substrate, adjacent S rTiO3There is nanoscale groove 1002 between single crystalline substrate.
The SrTiO3Substrate 100 has layered crystal structure, and layered crystal structure is by titanium dioxide (TiO2) layer with
Strontium oxide strontia (SrO) layer is alternately laminated to be formed.Specifically, the SrTiO3The lattice types of substrate 100 are tetragonal lattice.It is described
SrTiO3Substrate 100 is 0.3905 nanometer in the lattice constant of (100) crystal face.The SrTiO3Substrate 100 (100) crystal face with
The lattice mismatch of the FeSe single crystalline layer is 3% or so, which is conducive to (100) crystal face at this and grows
The FeSe single crystalline layer of high quality out.The SrTiO3The thickness of substrate 100 can be selected between 0.2 millimeter to 1.0 millimeters.It is described
SrTiO3The dielectric constant (10 with higher at low temperature of substrate 1004).The SrTiO3The dielectric with higher of substrate 100 is normal
Number is conducive to shield the interaction between carrier.For the ease of observing the high-temperature superconducting thin film using electronic transport measurement
The SrTiO of high resistant insulation may be selected in 10 superconducting transition temperature3Substrate 100.
The vacuum chamber 20 can be special vacuum annealing equipment, or subsequent growth FeSe high-temperature superconducting thin film
The reaction chamber of 104 equipment.Preferably, the present invention is using the equipment of growth FeSe high-temperature superconducting thin film 104 directly to described
SrTiO3Substrate 100 is made annealing treatment, and directly grows FeSe high-temperature superconducting thin film 104 so as to subsequent.Preferably, to described
SrTiO3When substrate 100 is made annealing treatment, the pressure of the vacuum chamber 20 is lower than 10-10mbar。
In the step S20, to the SrTiO3The method that substrate 100 heats is unlimited, can be by the vacuum chamber 20
Included heating device itself is heated, and special heating device also can be set.Referring to Fig. 1, the present invention first will be described
SrTiO3Substrate 100 is set to 103 surface of a heating element, then passes through first electrode 101 and second electrode 102 to the heating
Element 103 applies voltage, thus to the SrTiO3Substrate 100 is heated.Specifically, the heating element 103 can be gold
Belong to layer or silicon carbide layer etc., the first electrode 101 and second electrode 102 are metal holding electrode.101 He of first electrode
Second electrode 102 is respectively at both ends by the SrTiO3Substrate 100 and heating element 103 are fixed.Apply to the heating element 103
Voltage can be alternating current or direct current.
Present inventor discovery, by ultrahigh vacuum 900 DEG C can make this within 30 minutes or more annealed above
SrTiO3The surface of substrate 100 forms atomically flating.The step of thus eliminating existing boiling processing and acid processing,
It avoids and carries out the high temperature anneal in existing method in air and enter impurity.
Further, referring to fig. 2, in present inventor it has also been found that, by ultrahigh vacuum 1050 DEG C it is annealed above it
Afterwards, the groove 1002 of the polycrystalline circle substrate almost disappears, that is, the crystal boundary between adjacent single crystalline substrate heals completely, is formed former
Sub- grade contact.
However, present inventor also found, the above method treated SrTiO3Substrate 100 can not be directly used in
FeSe high-temperature superconducting thin film 104 is grown, this is because ultrahigh vacuum heat treatment leads to SrTiO3The a large amount of deoxidations of substrate 100.And
And the above method treated SrTiO3Substrate 100, it is conductive due to a large amount of deoxidations, be not suitable for growing and study
FeSe high-temperature superconducting thin film 104.
In order to grow and study FeSe high-temperature superconducting thin film 104, need to the above method treated SrTiO3Substrate 100
Oxygenating processing is carried out, to make the SrTiO3Substrate 100 is changed into insulator.Therefore, processing SrTiO3The method of substrate may be used also
To further comprise to the above method treated SrTiO3Substrate 100 carries out the step S30 of oxygenating processing, sees below.
Referring to Fig. 1 and 3-4, the embodiment of the present invention further provides for a kind of method for preparing FeSe superconductor 10 comprising
Following steps:
Step S10, by a SrTiO3Substrate 100 is placed in a vacuum chamber 20, and the pressure of the vacuum chamber 20 is lower than 10- 9Mbar, the SrTiO3100 surface of substrate is that non-atomic grade is smooth；
Step S20, by the SrTiO3Substrate 100 is heated to 900 DEG C or more, to the SrTiO3Substrate 100 anneal 30 minutes with
On；
Step S30, drops to 650 DEG C~800 DEG C for 20 temperature of vacuum chamber, is then passed through to the vacuum chamber 20 oxygenous
Atmosphere makes 20 pressure of vacuum chamber be maintained at 1 × 10-6Mbar~1 × 10-4Mbar, to the SrTiO after the annealing3Substrate 100 is mended
Oxygen is handled 10 minutes~30 minutes；And
Step S40, in the oxygenating treated SrTiO3100 surface of substrate grows FeSe high-temperature superconducting thin film 104.
In the step S30, the oxygen-containing atmosphere can be oxygen, air ozone.Annealing of the embodiment of the present invention and oxygenating
Vacuum chamber 20 be subsequent growth FeSe high-temperature superconducting thin film 104 equipment reaction chamber.Preferably, the embodiment of the present invention is adopted
Oxygenating is carried out with ozone.This is because to reach identical oxygenating effect, pressure required for oxygen and air is bigger, and amount is more
It is more.On the one hand, this can destroy the vacuum of vacuum chamber 20, cause intracavitary not carrying out molecular beam epitaxial growth.Another party
Face, for polycrystalline circle substrate, oxygenating will lead to crystal boundary and split again in the oxygen and air of High Voltage.
In the step S40, it can be existing any method that the method for growing FeSe high-temperature superconducting thin film 104 is unlimited.
Referring to Fig. 3, as the SrTiO3When substrate 100 is the polycrystalline circle substrate with nano-scale trenches 1002, growth
FeSe high-temperature superconducting thin film 104 is a polycrystalline circle superconducting thin film comprising the FeSe that multiple coplanar splicings are arranged and crystal orientation is different
Monocrystal thin films, and there is nanoscale gap 1042 corresponding with the groove 1002 between multiple FeSe monocrystal thin films.Referring to
Fig. 4, as the SrTiO3When substrate 100 is the polycrystalline circle substrate of no groove 1002, the FeSe high-temperature superconducting thin film 104 of growth
Multiple FeSe monocrystal thin films between crystal boundary heal completely, formed atomic level contact.That is, not having between two FeSe monocrystal thin films
It has the gap, to form an overall structure.
The following are specific embodiments of the present invention.
Embodiment 1
Firstly, by a SrTiO3Single crystalline substrate is placed in vacuum chamber, and the pressure of the vacuum chamber is < 10-9
Mbar, the SrTiO3Single crystalline substrate surface is that non-atomic grade is smooth.Secondly, by the SrTiO3Silicon is to 900 DEG C
~1000 DEG C, to the SrTiO3Substrate annealing 30 minutes or more.1 annealing temperature of embodiment be respectively 900 DEG C, 950 DEG C and
1000℃.Annealing time is respectively 30 minutes, 60 minutes, 75 minutes and 90 minutes.As shown in Figure 1, being used in the present embodiment
Silicon carbide heating layer passes through the DC heating SrTiO3Substrate.SrTiO referring to Fig. 5, after annealing3Substrate surface forms atom level
It is smooth.Annealing temperature is higher, and annealing time is longer, treated SrTiO3Substrate surface is more smooth.
However, the method for embodiment 1 treated SrTiO3It is thin can not to be directly used in growth FeSe high-temperature superconductor for substrate
Film, this is because ultrahigh vacuum heat treatment leads to SrTiO3The a large amount of deoxidations of substrate.Referring to Fig. 6, handled in the method for embodiment 1
Afterwards but non-oxygenating processing SrTiO3When substrate growth FeSe high-temperature superconducting thin film, only obtain the cluster of multiple dispersions, and
It is unable to get continuous FeSe single crystalline layer.Moreover, even if reducing SrTiO3Substrate growth temperature increases Se flow, or in Se gas
Anneal the SrTiO that can not all handle in non-oxygenating in atmosphere3Substrate surface obtains continuous FeSe single crystalline layer.
Embodiment 2
The embodiment of the present invention 2 and the method for embodiment 1 are essentially identical, the difference is that, embodiment 2 is on the basis of embodiment 1
On further to SrTiO3Substrate has carried out oxygenating processing, and using oxygenating treated SrTiO3Substrate growth FeSe high temperature is super
Lead film.
Specifically, to the SrTiO3The vacuum room temperature is dropped to 750 DEG C, so after annealing 60 minutes or more by substrate
The backward vacuum chamber is passed through oxygen-containing atmosphere, and pressure in vacuum tank is made to be maintained at 8 × 10-6Mbar, to the SrTiO after the annealing3Substrate
Oxygenating is carried out to handle 10 minutes.
2 oxygenating of embodiment treated SrTiO3Substrate is insulator, and is used directly for growth FeSe high-temperature superconductor
Film.Specifically, to the SrTiO after the annealing3After substrate carries out oxygenating processing, first stops being passed through oxygen-containing atmosphere, make the vacuum
The pressure of room is to drop to 10-9Mbar is hereinafter, and drop to 380 DEG C~420 DEG C for the vacuum room temperature.Then, respectively to the vacuum
Room is passed through a source Fe and a source Se, and the line ratio in the source Fe and the source Se is maintained at 1:10 between 1:20, the source Fe and Se
The growth temperature in source is kept between 1000 DEG C to 1100 DEG C between 130 DEG C to 150 DEG C, and the FeSe high-temperature superconductor is thin
The growth line of film is maintained at 0.25UC/min or so.Further, after having grown the FeSe high-temperature superconducting thin film, further
By the SrTiO3Substrate is annealed 20 hours to 30 hours between 450 DEG C to 550 DEG C.The purpose of the annealing is that removal is rich
Remaining Se, while improving the FeSe high-temperature superconducting thin film and the SrTiO3Bonding action between substrate, thus more advantageous
Obtaining stronger interface in the iron-based high-temperature superconductive film enhances superconductivity effects.
In the present embodiment, the line ratio in the source Fe and the source Se is maintained at 1:10.The SrTiO3Substrate temperature is kept
At 400 DEG C, the growth temperature in the source Fe and the source Se is kept at 1100 DEG C and 150 DEG C.It, will be described after growth
SrTiO3Substrate is annealed 70 minutes at 500 DEG C.Referring to Fig. 7-8, which is a single crystalline layer, thickness 1.2UC,
And the FeSe single crystalline layer and SrTiO3With the interface of an atomically flating between single crystalline substrate.
In the present embodiment, further in the FeSe high-temperature superconducting thin film far from the SrTiO3The surface of substrate grows one layer
FeTe single crystalline layer, as protective layer.With the boundary of an atomically flating between the FeTe single crystalline layer and the FeSe single crystalline layer
Face.
Embodiment 3
The embodiment of the present invention 3 and the method for embodiment 1 are essentially identical, the difference is that, the SrTiO of embodiment 33Substrate is double
Crystal boundary substrate.
Specifically, firstly, by a SrTiO3Twin boundary substrate is placed in vacuum chamber, and the pressure of the vacuum chamber is lower than 10- 9mbar.Secondly, the vacuum chamber is heated to 950 DEG C, to the SrTiO3Twin boundary substrate was in annealing 60 minutes.Referring to Fig. 9, this is not
The SrTiO of processing3Twin boundary substrate includes the SrTiO that two coplanar splicings are arranged and crystal orientation is different3Single crystalline substrate is adjacent
SrTiO3With 80 nanometers of width between single crystalline substrate, the groove that 0.6 nanometer of depth, and each SrTiO3Single crystalline substrate surface is
Non-atomic grade is smooth.SrTiO referring to Figure 10, after annealing3Twin boundary substrate surface forms atomically flating, but adjacent
Groove between single crystalline substrate still has, about 15 nanometers wide, 1 nanometer of depth.The method of same embodiment 3 treated SrTiO3
Substrate can not be directly used in growth FeSe high-temperature superconducting thin film.
Embodiment 4
The embodiment of the present invention 4 and the method for embodiment 3 are essentially identical, the difference is that, embodiment 4 is on the basis of embodiment 3
On further to SrTiO3Substrate has carried out oxygenating processing, and using oxygenating treated SrTiO3Substrate growth FeSe high temperature is super
Lead film.
In the present embodiment, to the SrTiO3Twin boundary substrate drops the vacuum room temperature after annealing 60 minutes or more
To 750 DEG C, it then is passed through ozone to the vacuum chamber, being maintained at pressure in vacuum tank is 1 × 10-5Mbar, after the annealing
SrTiO3Twin boundary substrate carries out oxygenating and handles 15 minutes.
4 oxygenating of embodiment treated SrTiO3Twin boundary substrate is insulator, and is used directly for growth FeSe high
Temperature superconductive film.Specifically, using the method for the growth FeSe high-temperature superconducting thin film of embodiment 2 in SrTiO3Twin boundary substrate table
It looks unfamiliar long FeSe high-temperature superconducting thin film.Referring to Figure 11, the FeSe high-temperature superconducting thin film of the present embodiment growth is a twin boundary superconduction
Film.The FeSe twin boundary superconducting thin film includes two coplanar splicing settings and the different FeSe monocrystal thin films of crystal orientation, and this two
A FeSe monocrystal thin films have gap.The FeSe monocrystal thin films and SrTiO3With an atomically flating between single crystalline substrate
Interface.After growing FeSe, by the SrTiO3Substrate is annealed 70 minutes at 500 DEG C.Referring to Figure 12, the FeSe twin crystal of growth
After annealing, there is apparent dark farmland, and FeSe monocrystal thin films decompose near crystal boundary along dark farmland in boundary's superconducting thin film.
In the present embodiment, further in the FeSe high-temperature superconducting thin film far from the SrTiO3The surface of substrate grows one layer
FeTe single crystalline layer, as protective layer.With an atomically flating between the FeTe single crystalline layer and the FeSe monocrystal thin films
Interface.
Embodiment 5
The embodiment of the present invention 5 and the method for embodiment 3 are essentially identical, the difference is that, to the SrTiO3Twin boundary substrate exists
The temperature of vacuum chamber annealing is 1000 DEG C, and annealing time is 60 minutes.SrTiO referring to Figure 13, after the present embodiment annealing3Twin crystal
Boundary's substrate surface forms atomically flating, but the groove between adjacent single crystalline substrate still has.
Embodiment 6
The embodiment of the present invention 6 and the method for embodiment 4 are essentially identical, the difference is that, to the SrTiO3Twin boundary substrate exists
The temperature of vacuum chamber annealing is 1000 DEG C, and annealing time is 60 minutes.Referring to Figure 14, the FeSe high-temperature superconductor of the present embodiment growth
Film is a twin boundary superconducting thin film, and still has clear gap between two FeSe monocrystal thin films.Referring to Figure 15, this reality
It applies in example, even if the FeSe of raw 10UC, can only also fill SrTiO after 450 DEG C of annealing3The part of trench of twin boundary substrate.
The present embodiment further tests the R-T characteristic of the FeSe high-temperature superconducting thin film of preparation.Referring to Figure 33-34,
Gap or crystal boundary two sides can observe zero resistance R1 and R2 in 10K or less, but across grain boundary resistance Rc is still in 1.8K
2Ohm.Resistance Rc across crystal boundary is primarily due to still cause with clear gap between two FeSe monocrystal thin films.
Embodiment 7
The embodiment of the present invention 7 and the method for embodiment 3 are essentially identical, the difference is that, to the SrTiO3Twin boundary substrate exists
The temperature of vacuum chamber annealing is 1050 DEG C or more.
Specifically, firstly, by a SrTiO3Twin boundary substrate is placed in vacuum chamber, and the pressure of the vacuum chamber is lower than 10- 9mbar.Secondly, the vacuum chamber is heated to 1050 DEG C or more, to the SrTiO3Twin boundary substrate was at annealing 10 minutes or more.It is real
Applying 7 annealing temperature of example is respectively 1050 DEG C, 1100 DEG C and 1200 DEG C.Annealing time is respectively 10 minutes, 20 minutes, 30 points
Clock, 60 minutes and 90.Experiment discovery is annealed 10 minutes or more at 1050 DEG C can make the crystal boundary between adjacent single crystalline substrate complete
Full healing forms atomic level contact, and substrate surface forms atomically flating.Referring to Figure 16, after the present embodiment annealing
SrTiO3Twin boundary substrate surface forms atomically flating, and the groove between adjacent single crystalline substrate almost disappears, that is, adjacent list
Crystal boundary between brilliant substrate heals completely, forms atomic level contact.Due to SrTiO3Twin boundary substrate gradually loses at 1050 DEG C
Oxygen, resistance reduce, and temperature can increase, and are easy to cause the risk of fracture.And annealing time at 1050 DEG C is reduced, substrate can be reduced
Lead to the risk of fracture since temperature is excessively high.It is therefore preferred that annealing time is less than or equal to 60 minutes.
Embodiment 8
The embodiment of the present invention 8 and the method for embodiment 7 are essentially identical, the difference is that, embodiment 8 is on the basis of embodiment 7
On further to SrTiO3Substrate has carried out oxygenating processing, and using oxygenating treated SrTiO3Substrate growth FeSe high temperature is super
Lead film.
Specifically, firstly, by a SrTiO3Twin boundary substrate is placed in vacuum chamber, and the pressure of the vacuum chamber is lower than 10- 9mbar.Secondly, the vacuum chamber is heated to 1050 DEG C, to the SrTiO3Twin boundary substrate was in annealing 60 minutes.Then using real
The method for applying example 2 carries out oxygenating processing and growth FeSe high-temperature superconducting thin film.Referring to Figure 17, the FeSe high temperature of the present embodiment growth
Superconducting thin film is a twin boundary superconducting thin film, thickness 1.2UC, and the crystal boundary between two FeSe monocrystal thin films heals completely,
Form atomic level contact.That is, there is no gap between two FeSe monocrystal thin films, to form an overall structure.The FeSe monocrystalline
Film and SrTiO3With the interface of an atomically flating between single crystalline substrate.After growing FeSe, by the SrTiO3Substrate
It anneals 60 minutes at 490 DEG C.Referring to Figure 18, after annealing, there is apparent dark farmland in the FeSe twin boundary superconducting thin film of growth, and
FeSe monocrystal thin films decompose near crystal boundary along dark farmland.Referring to Figure 19-21, the position of two FeSe single crystalline layers contact has
Apparent crystal boundary, and the FeSe single crystalline layer of the crystal boundary two sides has different crystal orientation.
In the present embodiment, further in the FeSe high-temperature superconducting thin film far from the SrTiO3The surface of substrate grows one layer
FeTe single crystalline layer, as protective layer.With an atomically flating between the FeTe single crystalline layer and the FeSe monocrystal thin films
Interface.
The present embodiment further tests the R-T characteristic of the FeSe high-temperature superconducting thin film of preparation.Referring to Figure 35-36,
Gap or crystal boundary unilateral side can observe zero resistance R1 in 12K or less, but the resistance Rc across crystal boundary is in 1.8K
20mOhm.Resistance Rc across crystal boundary, which is primarily due to two FeSe monocrystal thin films, to be caused near crystal boundary along the decomposition of dark farmland.Phase
Compared with the sample of embodiment 6, the sample of embodiment 8 is obviously reduced across the resistance Rc of crystal boundary.
Embodiment 9
The embodiment of the present invention 9 and the method for embodiment 8 are essentially identical, the difference is that, the oxygenating temperature of embodiment 8 is 750
DEG C, and the oxygenating temperature of embodiment 9 is 680 DEG C.Referring to fig. 22, the FeSe high-temperature superconducting thin film of the present embodiment growth is a twin crystal
Boundary's superconducting thin film, thickness 1.2UC, and the crystal boundary between two FeSe monocrystal thin films heals completely, forms atomic level contact.It is raw
After long FeSe, by the SrTiO3Substrate is annealed 60 minutes at 450 DEG C.Referring to fig. 23, the FeSe twin boundary superconduction of growth
Film after annealing, does not observe light/dark farmland, but FeSe monocrystal thin films decompose still near crystal boundary along dark farmland.
Embodiment 10
The embodiment of the present invention 10 and the method for embodiment 3 are essentially identical, the difference is that, by the SrTiO3Twin boundary substrate exists
950 DEG C are annealed 40 minutes and then vacuum chamber are heated to 1050 DEG C of re-annealings 20 minutes.That is, embodiment 10 respectively includes not
Twice annealing under synthermal.Referring to fig. 24, the SrTiO after 1050 DEG C of the present embodiment annealing3Twin boundary substrate surface forms original
Sub- grade is smooth, and the crystal boundary between adjacent single crystalline substrate heals completely, forms atomic level contact.Embodiment 10 is first at 950 DEG C
It is increased within preannealing 40 minutes 1050 DEG C of annealing again, primarily to reducing the difficulty for directly heating to 1050 DEG C and maintaining ultrahigh vacuum
Degree.
Embodiment 11
The embodiment of the present invention 11 and the method for embodiment 10 are essentially identical, the difference is that, embodiment 11 is in embodiment 10
On the basis of further to SrTiO3Substrate has carried out oxygenating processing, and using oxygenating treated SrTiO3Substrate growth FeSe high
Temperature superconductive film.
Specifically, using the method for the growth FeSe high-temperature superconducting thin film of embodiment 2 in SrTiO3Twin boundary substrate surface
Grow FeSe high-temperature superconducting thin film.Referring to fig. 25, the FeSe high-temperature superconducting thin film of the present embodiment growth is that a twin boundary superconduction is thin
Film, and the crystal boundary between two FeSe monocrystal thin films heals completely, forms atomic level contact.After growing FeSe, by institute
State SrTiO3Substrate is annealed 60 minutes at 430 DEG C.Referring to fig. 26, the FeSe twin boundary superconducting thin film of growth after annealing, is not seen
Light/dark farmland is measured, but FeSe monocrystal thin films decompose still near crystal boundary along dark farmland.
Embodiment 12
The embodiment of the present invention 12 and the method for embodiment 7 are essentially identical, the difference is that, using described in AC electric-heating
SrTiO3Twin boundary substrate.Referring to fig. 27, the SrTiO after the present embodiment annealing3Twin boundary substrate surface forms atomically flating,
And the groove between adjacent single crystalline substrate almost disappears.
Experiment also found, using SrTiO described in AC electric-heating3When substrate, the SrTiO3Substrate is not easy to break.And it uses
SrTiO described in DC heating3When substrate, the SrTiO3Substrate is easy to be broken.This is because when using DC heating, it should
SrTiO3The substrate Lacking oxygen that deoxidation generates at high temperature is deposited in cathode side, leads to the SrTiO3Substrate local temperature is excessively high,
It is easily broken off.When using exchange heating, the SrTiO3The substrate Lacking oxygen that deoxidation generates at high temperature is evenly distributed on SrTiO3
In substrate, therefore, the SrTiO3Substrate temperature distribution is also very uniform, not easy to break.
In addition, due to the SrTiO using DC heating processing3Lacking oxygen in substrate is unevenly distributed, in subsequent oxygenating
After processing, SrTiO3Oxygen element distribution in substrate is also less uniform.Long in the process of subsequent growth FeSe, Lacking oxygen is excessive
Place will lead to the FeSe film that cannot get high quality.Moreover, in the case where being handled using DC heating, the SrTiO of negative side3
Substrate still remains conductive possibility after oxygenating, influences the subsequent research to FeSe film superconductivity.However, being added using exchange
The SrTiO of heat treatment3Lacking oxygen in substrate is evenly distributed, in subsequent oxygenating treatment process, SrTiO3Substrate can be abundant
Oxygenating.
Embodiment 13
The embodiment of the present invention 13 and the method for embodiment 12 are essentially identical, the difference is that, embodiment 13 is in embodiment 12
On the basis of further to SrTiO3Substrate has carried out oxygenating processing, and using oxygenating treated SrTiO3Substrate growth FeSe high
Temperature superconductive film.
Specifically, using the method for the growth FeSe high-temperature superconducting thin film of embodiment 2 in SrTiO3Twin boundary substrate surface
Grow FeSe high-temperature superconducting thin film.Referring to fig. 28, the FeSe high-temperature superconducting thin film of the present embodiment growth is that a twin boundary superconduction is thin
Film, and the crystal boundary between two FeSe monocrystal thin films heals completely, forms atomic level contact.After growing FeSe, by institute
State SrTiO3Substrate is annealed 60 minutes at 490 DEG C.Referring to fig. 29, the FeSe twin boundary superconducting thin film of growth after annealing, crystal boundary
There is bright farmland in two sides FeSe film, and FeSe monocrystal thin films do not decompose, but grain boundaries swell, about 1 nanometer higher than two sides.
The present embodiment further tests the R-T characteristic of the FeSe high-temperature superconducting thin film of preparation.Referring to Figure 37, gap
Or the resistance R1 and R2 of crystal boundary two sides, and the resistance Rc across crystal boundary can observe zero-resistance phenomenon in 10K or less.Across crystalline substance
The resistance Rc on boundary can observe zero-resistance phenomenon, be due to FeSe twin boundary superconducting thin film after annealing, FeSe monocrystal thin films
Not occurring decomposing causes.
Comparative example 1
Comparative example 1 of the present invention and the method for embodiment 1 are essentially identical, the difference is that, annealing temperature is 650 DEG C.Referring to figure
30, using method treated the SrTiO of comparative example 13It is smooth that substrate surface remains as non-atomic grade, and the SrTiO3Substrate without
Method is for growing FeSe high-temperature superconducting thin film.
Comparative example 2
Comparative example 2 of the present invention and the method for embodiment 3 are essentially identical, the difference is that, annealing temperature is 650 DEG C.Referring to figure
31, using method treated the SrTiO of comparative example 23It is smooth that twin boundary substrate surface remains as non-atomic grade, two monocrystalline
SrTiO380 nanometers of groove width between substrate, 1 nanometer of depth, and the SrTiO3Twin boundary substrate is not used to growth FeSe
High-temperature superconducting thin film.
Comparative example 3
Comparative example 3 of the present invention handles SrTiO using the method for the Chinese patent application of Publication No. CN105679647A3It is double
Crystal boundary substrate.
Specifically, two SrTiO with burnishing surface are provided3Twin boundary substrate is placed sequentially in acetone, isopropanol, surpasses
After each ultrasonic five minutes in pure water are cleaned, by SrTiO3After twin boundary substrate hot bath is impregnated 1 hour, being placed on concentration is
It is impregnated 45 minutes in 10% hot hydrochloric acid (HCl), obtains two pretreated SrTiO3Twin boundary substrate.It is pretreated by two
SrTiO3Twin boundary substrate is laminated in pure water, makes two pretreated SrTiO3The burnishing surface of twin boundary substrate is opposite and is overlapped
Setting obtains a laminate structure.Above-mentioned laminate structure is placed in high temperature furnace, in the oxygen atmosphere of about atmospheric pressure
It after annealing 3 hours at a temperature of lower 1080 DEG C, is separated, obtains two SrTiO with atomically flating surface3Twin boundary
Substrate.Referring to Figure 32, the SrTiO3Surface of the twin boundary substrate with atomically flating, but two monocrystalline SrTiO3Substrate it
Between groove width be 80 nanometers, depth be 10 nanometers.That is, the method for comparative example 3 does not simply fail to make two monocrystalline SrTiO3Lining
Groove between bottom disappears, and makes the depth down of the groove instead.
Further, using the SrTiO with atomically flating surface3Twin boundary substrate growth FeSe high-temperature superconductor is thin
Film.The FeSe high-temperature superconducting thin film of growth is two independent FeSe monocrystal thin films.That is, quilt between two FeSe monocrystal thin films
Gap isolation, can not form continuous crystal boundary.
In addition, those skilled in the art can also do other variations in spirit of that invention, these are spiritual according to the present invention
The variation done should be all included in scope of the present invention.
Claims (10)
1. a kind of SrTiO3The preparation method of polycrystalline circle substrate, which is characterized in that itself the following steps are included:
By a untreated SrTiO3Polycrystalline circle substrate is placed in a vacuum chamber, and the pressure of the vacuum chamber is lower than 10-9Mbar,
In, the untreated SrTiO3Polycrystalline circle substrate includes the SrTiO that multiple coplanar splicings are arranged and crystal orientation is different3Single crystalline substrate, phase
Adjacent SrTiO3There is groove, and each SrTiO between single crystalline substrate3Single crystalline substrate surface is that non-atomic grade is smooth；And
By the untreated SrTiO3Polycrystalline circle silicon is to 1050 DEG C or more, to the untreated SrTiO3Polycrystalline circle substrate
Annealing 10 minutes or more.
2. SrTiO as described in claim 13The preparation method of polycrystalline circle substrate, which is characterized in that described untreated
SrTiO3The method of polycrystalline circle silicon are as follows: by the untreated SrTiO3Polycrystalline circle substrate is set to a heating element table
Then face applies voltage to the heating element by first electrode and second electrode.
3. SrTiO as claimed in claim 23The preparation method of polycrystalline circle substrate, which is characterized in that pass through first electrode and
Two electrodes apply alternating current to the heating element.
4. SrTiO as claimed in claim 23The preparation method of polycrystalline circle substrate, which is characterized in that pass through first electrode and
Two electrodes apply direct current to the heating element.
5. SrTiO as described in claim 13The preparation method of polycrystalline circle substrate, which is characterized in that untreated to this
SrTiO3Polycrystalline circle substrate is 30 minutes or more annealed above at 1050 DEG C.
6. SrTiO as described in claim 13The preparation method of polycrystalline circle substrate, which is characterized in that this is untreated
SrTiO3Polycrystalline circle silicon is to before 1050 DEG C or more, first by the untreated SrTiO3Polycrystalline circle substrate is preheated to 900
DEG C~1000 DEG C, and kept for 30 minutes or more.
7. SrTiO as described in claim 13The preparation method of polycrystalline circle substrate, which is characterized in that untreated to this
SrTiO3After polycrystalline circle substrate annealing 10 minutes or more, further comprise: the vacuum room temperature dropped to 650 DEG C~800 DEG C,
Then it is passed through oxygen-containing atmosphere to the vacuum chamber, pressure in vacuum tank is made to be maintained at 1 × 10-6Mbar~1 × 10-4Mbar, to the annealing
SrTiO afterwards3Polycrystalline circle substrate carries out oxygenating and handles 10 minutes~30 minutes.
8. SrTiO as claimed in claim 73The preparation method of polycrystalline circle substrate, which is characterized in that the oxygen-containing atmosphere is smelly
Oxygen.
9. a kind of SrTiO3Polycrystalline circle substrate comprising: the SrTiO that multiple coplanar splicings are arranged and crystal orientation is different3Single crystalline substrate,
It is characterized in that, adjacent S rTiO3Crystal boundary between single crystalline substrate heals completely, forms atomic level contact, and each SrTiO3It is single
Brilliant substrate surface is atomically flating.
10. SrTiO as claimed in claim 93Polycrystalline circle substrate, which is characterized in that each SrTiO3Single crystalline substrate includes multiple
Lacking oxygen, so that the SrTiO3Polycrystalline circle substrate is an electric conductor.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111411400A (en) * | 2020-04-17 | 2020-07-14 | 中国电子科技南湖研究院 | Hot isostatic pressing connection method of high-purity semiconductor single crystal |
| WO2020248517A1 (en) * | 2019-06-14 | 2020-12-17 | 清华大学 | Method for treating srtio3 single grain boundary or multiple grain boundary substrate by means of ultra-high vacuum annealing, and method for preparing fese superconducting film |
| CN112176415A (en) * | 2020-09-23 | 2021-01-05 | 北京大学 | Method for obtaining single titanium oxide terminated insulating strontium titanate (001) surface |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03242320A (en) * | 1990-02-16 | 1991-10-29 | Nippon Telegr & Teleph Corp <Ntt> | Oxide superconductor thin film |
| JPH0499078A (en) * | 1990-08-06 | 1992-03-31 | Komatsu Ltd | Formation of thin film and manufacture of superconducting device using same |
| JP2002280380A (en) * | 2001-03-19 | 2002-09-27 | Japan Science & Technology Corp | Method of forming film for semiconductor device |
| CN1718561A (en) * | 2004-07-06 | 2006-01-11 | 中国科学院合肥物质科学研究院 | Barium strontium titanate film material and preparation method |
| US20090247413A1 (en) * | 2008-03-27 | 2009-10-01 | Mariko Hayashi | Oxide superconductor and method of fabricating same |
| CN103184513A (en) * | 2013-03-13 | 2013-07-03 | 清华大学 | Preparation method of high-temperature superconducting thin film |
| WO2013108507A1 (en) * | 2012-01-20 | 2013-07-25 | 富士電機株式会社 | Manganese oxide thin film and oxide laminate |
| CN104947192A (en) * | 2015-05-25 | 2015-09-30 | 中国科学院上海微***与信息技术研究所 | Preparation method of perovskite type SrIrO3 single crystal film material |
| CN105161217A (en) * | 2015-07-07 | 2015-12-16 | 中国科学院上海微***与信息技术研究所 | Perovskite type Sr2IrO4 monocrystalline thin film material preparation method |
| CN105679647A (en) * | 2015-12-31 | 2016-06-15 | 清华大学 | Preparation method for substrates with atomic-scale flat surfaces |
-
2019
- 2019-06-14 CN CN201910518122.2A patent/CN110265191B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03242320A (en) * | 1990-02-16 | 1991-10-29 | Nippon Telegr & Teleph Corp <Ntt> | Oxide superconductor thin film |
| JPH0499078A (en) * | 1990-08-06 | 1992-03-31 | Komatsu Ltd | Formation of thin film and manufacture of superconducting device using same |
| JP2002280380A (en) * | 2001-03-19 | 2002-09-27 | Japan Science & Technology Corp | Method of forming film for semiconductor device |
| CN1718561A (en) * | 2004-07-06 | 2006-01-11 | 中国科学院合肥物质科学研究院 | Barium strontium titanate film material and preparation method |
| US20090247413A1 (en) * | 2008-03-27 | 2009-10-01 | Mariko Hayashi | Oxide superconductor and method of fabricating same |
| WO2013108507A1 (en) * | 2012-01-20 | 2013-07-25 | 富士電機株式会社 | Manganese oxide thin film and oxide laminate |
| CN103184513A (en) * | 2013-03-13 | 2013-07-03 | 清华大学 | Preparation method of high-temperature superconducting thin film |
| CN104947192A (en) * | 2015-05-25 | 2015-09-30 | 中国科学院上海微***与信息技术研究所 | Preparation method of perovskite type SrIrO3 single crystal film material |
| CN105161217A (en) * | 2015-07-07 | 2015-12-16 | 中国科学院上海微***与信息技术研究所 | Perovskite type Sr2IrO4 monocrystalline thin film material preparation method |
| CN105679647A (en) * | 2015-12-31 | 2016-06-15 | 清华大学 | Preparation method for substrates with atomic-scale flat surfaces |
| CN105679647B (en) * | 2015-12-31 | 2018-06-29 | 清华大学 | The preparation method of substrate with atomically flating surface |
Non-Patent Citations (2)
| Title |
|---|
| M KAWASAKI ETC: "Atomic Control of th SrTiO3 Crystal Surface", 《SCIENCE》 * |
| 王萌等: "《SrTiO3(001)衬底上单层FeSe超导薄膜的》", 《物理学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020248517A1 (en) * | 2019-06-14 | 2020-12-17 | 清华大学 | Method for treating srtio3 single grain boundary or multiple grain boundary substrate by means of ultra-high vacuum annealing, and method for preparing fese superconducting film |
| CN111411400A (en) * | 2020-04-17 | 2020-07-14 | 中国电子科技南湖研究院 | Hot isostatic pressing connection method of high-purity semiconductor single crystal |
| CN112176415A (en) * | 2020-09-23 | 2021-01-05 | 北京大学 | Method for obtaining single titanium oxide terminated insulating strontium titanate (001) surface |
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