CN110257912A - Single-crystal strontium titanate substrate base and preparation method thereof with atom level step structure - Google Patents
Single-crystal strontium titanate substrate base and preparation method thereof with atom level step structure Download PDFInfo
- Publication number
- CN110257912A CN110257912A CN201910644631.XA CN201910644631A CN110257912A CN 110257912 A CN110257912 A CN 110257912A CN 201910644631 A CN201910644631 A CN 201910644631A CN 110257912 A CN110257912 A CN 110257912A
- Authority
- CN
- China
- Prior art keywords
- substrate base
- preparation
- ultrasonic cleaning
- strontium
- strontium titanates
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
- C30B29/32—Titanates; Germanates; Molybdates; Tungstates
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/02—Heat treatment
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/08—Etching
- C30B33/10—Etching in solutions or melts
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Cleaning Or Drying Semiconductors (AREA)
Abstract
The invention discloses a kind of preparation methods of single-crystal strontium titanate substrate base with atom level step structure.The preparation method includes: that untreated strontium titanates substrate base is carried out first time ultrasonic cleaning；Strontium titanates substrate base after being cleaned for the first time with ammonium fluoride-buffered hydrofluoric acid solution corrosion；Gained strontium titanates substrate base is made annealing treatment under temperature flowing oxygen atmosphere；Strontium titanates substrate base after annealing is subjected to second of ultrasonic cleaning, obtains the single-crystal strontium titanate substrate base with atom level step structure；And the resulting single-crystal strontium titanate substrate base with atom level step structure is subjected to slice.Titanium-oxygen that the preparation method enables to the corrosion of single-crystal strontium titanate substrate base orientability to provide step structure terminates face, and pH value is suitable for, and surface presentation is apparent step-like, and surface Root Mean Square roughness is low, and entire ledge surface, which has no corrosion hole, to be occurred.
Description
Technical field
The present invention relates to a kind of substrate material technical fields, especially with regard to a kind of monocrystalline with atom level step structure
Strontium titanates substrate base and preparation method thereof.
Background technique
Strontium titanates (SrTiO3) substrate base is most wide one of the outstanding HTS single crystals substrate of current application.Numerous
In superconductor (such as yttrium barium copper oxide), ferroelectricity or the application of more ferroelectric material films (such as bismuth ferrite) high temperature functional materials, strontium titanates
Monocrystal chip has preferable lattice match, no twin structure, and physics, good mechanical performance, therefore, strontium titanate monocrystal chip
There is extremely important application value in science, production activity.The property and surface shape of strontium titanates substrate material are to film
Characteristic have a great impact, strontium-oxygen and titanium-oxygen staggeredly or both possess different contact surfaces to preparation in above-mentioned superconduction material
Material, ferroelectric thin film mass action are very big.Prepare the metatitanic acid in atom level step flatness and nanoscale r.m.s. roughness
Strontium substrate surface can provide the polarity and preferable growth kinetics condition needed to film material with function.Therefore, it obtains former
The strontium titanates substrate surface of sub- grade step is extremely important for superconduction, iron film.
The prior art does not occur high, the reproducible strontium titanate monocrystal chip atom level ledge surface of system, quality also
Preparation method.Mainly by strontium-oxygen and titanium-, oxygen is staggered to form dynamics terminates face on untreated strontium titanates substrate base surface,
It is easy that film material with function is made to show island growth mode, more film growth defect can be brought.In the market and academia
Emerge the strontium titanates substrate base surface treatment method of some chemistry, physics mode.
With it is more be but the acidic value and ionic species of this method buffer using ammonium fluoride buffer chemical method
How to configure and be related to seldom, therefore does not explore the buffered etch liquid condition and chemical time of optimization, so that
The strontium titanates substrate base surface prepared often will appear coralloid ledge surface, and defect hole is obvious, high quality
Function film can there are crystal boundaries or nonideal polycrystalline state in fault location, while easily occurring the island growth of film at hole
Mode, rather than layer by layer growth mode can have screw dislocation in island growth mode, these are all that high quality function film will be kept away
Exempt from.
Another processing method is the physics mode using high annealing, and this method is difficult that temperature is relied on to control substrate merely
Surface atom is to overcome own dynamics potential barrier and reconstructing surface, therefore this method is hardly formed the atom level of micron order large area
Step, and the unknown object of white tip-like is often precipitated in surface, is less useful for the growth of high quality function film.
The present invention proposes a kind of preparation method of single-crystal strontium titanate substrate base surface atom grade step structure.This method knot
Chemically and physically two kinds of film surface binding modes are closed, the ammonium fluoride buffer for optimizing pH value, and strict control are matched out
Reaction time；After chemical processing, the processing of temperature flowing oxygen atmosphere annealing is carried out at once, and strict control annealing time is had
The atom level step strontium titanates substrate surface for thering is single titanium-oxygen to terminate.
The information disclosed in the background technology section is intended only to increase the understanding to general background of the invention, without answering
When being considered as recognizing or imply that the information constitutes the prior art already known to those of ordinary skill in the art in any form.
Summary of the invention
The purpose of the present invention is to provide a kind of preparations of single-crystal strontium titanate substrate base with atom level step structure
Method, the titanium-oxygen for enabling to the corrosion of single-crystal strontium titanate substrate base orientability to provide step structure terminate face, and acid
Basicity is suitable for that can be avoided the appearance of etch pit.
To achieve the above object, the present invention provides a kind of single-crystal strontium titanate substrate bases with atom level step structure
Preparation method, comprising:
(1) untreated strontium titanates substrate base is subjected to first time ultrasonic cleaning；
(2) the strontium titanates substrate base after being cleaned for the first time with ammonium fluoride-buffered hydrofluoric acid solution corrosion；
(3) strontium titanates substrate base obtained by step (2) is made annealing treatment under temperature flowing oxygen atmosphere；
(4) the strontium titanates substrate base after annealing is subjected to second of ultrasonic cleaning, obtained with atom level platform
The single-crystal strontium titanate substrate base of stage structure；And
(5) the resulting single-crystal strontium titanate substrate base with atom level step structure of step (4) is subjected to slice.
In a preferred embodiment, above-mentioned untreated strontium titanates substrate base surface is by chemically mechanical polishing
, the surface Root Mean Square roughness of strontium titanates substrate base is in 2nm or less.
In a preferred embodiment, in step (1), the first time ultrasonic cleaning includes three steps, described
Cleaning step is successively: firstly, untreated strontium titanates substrate base ultrasonic wave in acetone soln is cleaned, acetone is molten
The liquid ultrasonic cleaning time is 5~30min, preferably 10min；Then, the strontium titanates substrate base after acetone soln being cleaned exists
Ultrasonic wave is cleaned in ethanol solution, and the ethanol solution ultrasonic cleaning time is 5~30min, preferably 10min；Finally, by second
Strontium titanates substrate base after alcoholic solution cleaning carries out ultrasonic cleaning in deionized water, and the deionized water ultrasonic cleaning time is
5~30min, preferably 10min.
In above-mentioned steps, the remaining organic matter of substrate surface is cleaned using acetone and ethyl alcohol, such as grease, rosin and wax.
In a preferred embodiment, in step (2), the pH value of the ammonium fluoride-buffered hydrofluoric acid solution is 4.5-
5.5。
Select pH value for ammonium fluoride-buffered hydrofluoric acid solution of 4.5-5.5, step structure is provided in orientability corrosion
Titanium-oxygen terminates face, and pH value is suitable for, and can be avoided the appearance of etch pit.
In a preferred embodiment, the preparation method of the ammonium fluoride-buffered hydrofluoric acid solution is: by ammonium hydroxide (NH3-
H2O soda acid mixed configuration) is carried out with HF, or by ammonium fluoride (NH4F it) is formed with HF mixed configuration.
In a preferred embodiment, in step (2), ammonium fluoride-buffered hydrofluoric acid solution etching time is 30~
45s。
If etching time is lower than 30s, single-crystal strontium titanate substrate base surface is not in atom level step；When corrosion
Between if it exceeds 45s, even if surface also has out in the case where atom level step occurs in single-crystal strontium titanate substrate base surface
Now corrode hole.
In a preferred embodiment, in step (3), the condition of the annealing is: by strontium titanates substrate base
It being placed in vacuum environment, is passed through the oxygen of flowing, control temperature within the scope of 950 DEG C~1100 DEG C, annealing time is 0.5~
2h, preferred annealing time are 1h.
If above-mentioned annealing time is too long, the surface reconstruction of single-crystal strontium titanate substrate base is excessive, will always there is atomic energy
Higher kinetic barrier is crossed, other shapes of body structure surface is formed.
If etching time is lower than 30s, and subsequent 950 DEG C of annealing 1h condition in addition, gained substrate in above-mentioned steps (2)
Surface also will appear smooth step-like, but be the step of half atom layer height, illustrate strontium-oxygen terminates surface corrosion and is inadequate
Thoroughly, there is a small amount of strontium-oxygen and the simultaneous surface of titanium-oxygen.
In a preferred embodiment, it may further comprise: and spend the strontium titanates substrate base after buffering corrosion
Ionized water is made annealing treatment again after being cleaned by ultrasonic.
Above-mentioned the advantages of being cleaned by ultrasonic with deionized water, is: after buffer processing, the surface of single-crystal strontium titanate substrate base
Inevitably remain ion NH4 +、F-Deng, with deionized water be cleaned by ultrasonic dry up, can prevent annealing high temperature when ion with
Single-crystal strontium titanate substrate reacts again.
In a preferred embodiment, the time of the deionized water ultrasonic cleaning is 5~30min, preferably
10min。
In a preferred embodiment, in step (4), second of ultrasonic cleaning includes three steps, described
Cleaning step is successively: firstly, ultrasonic wave cleans in acetone soln by the strontium titanates substrate base after annealing, third
The ketone solution ultrasonic cleaning time is 5~30min, preferably 10min；Then, the strontium titanates substrate base after acetone soln being cleaned
Piece ultrasonic wave in ethanol solution is cleaned, and the ethanol solution ultrasonic cleaning time is 5~30min, preferably 10min；Finally,
Strontium titanates substrate base after ethanol solution is cleaned carries out ultrasonic cleaning in deionized water, when deionized water is cleaned by ultrasonic
Between be 5~30min, preferably 10min.
Another object of the present invention is to provide have atom made from more than one described in any item preparation methods
The single-crystal strontium titanate substrate base of grade step structure.
Compared with prior art, the invention has the following beneficial effects:
(1) present invention uses pH value to handle for 4.5~5.5 ammonium fluoride buffered hydrofluoric acid solution and suitable annealing steps
Afterwards, the titanyl for enabling to the corrosion of single-crystal strontium titanate substrate base orientability to provide step structure terminates face, and pH value
It is suitable for that surface is presented apparent step-like (0.35nm, 1 atom layer height of about strontium titanates), and entire ledge surface is simultaneously
Corrosion-free hole occurs, and surface Root Mean Square roughness is about 0.13nm；Compared to untreated and only buffered through hydrofluoric acid ammonium fluoride
The substrate surface of single-crystal strontium titanate substrate base at liquid, this method processing shows desired step structure, and surface quality is non-
Chang Hao does not have hole appearance at step center, and surface Root Mean Square roughness is low, is conducive to the growth of high quality function film.
(2) annealing time is suitable in the present invention, and the surface reconstruction that not will cause single-crystal strontium titanate substrate base is excessive, can
Atomic energy is avoided to cross the body structure surface that higher kinetic barrier forms non-step shape.
(3) after pH value is 4.5~5.5 ammonium fluoride buffered hydrofluoric acid solution and the processing of suitable annealing steps, institute can be made
Obtain single-crystal strontium titanate substrate base
(4) present invention buffer processing after with deionized water be cleaned by ultrasonic dry up, it is capable of washing fall single-crystal strontium titanate substrate
The ion NH remained on surface of substrate4 +、F-Deng, prevent annealing high temperature when ion reacted again with single-crystal strontium titanate substrate.
Detailed description of the invention
Fig. 1 is the preparation flow figure of the single-crystal strontium titanate substrate base with atom level step structure according to the present invention.
Fig. 2 is the two-dimensional appearance figure on untreated single-crystal strontium titanate substrate base surface.
Fig. 3 is the Roughness analysis figure on untreated single-crystal strontium titanate substrate base surface.
Fig. 4 is the three-dimensional appearance figure on untreated single-crystal strontium titanate substrate base surface.
Fig. 5 is comparative example 6 merely through the two of hydrofluoric acid-ammonium fluoride buffer processing single-crystal strontium titanate substrate base surface
Tie up shape appearance figure.
Fig. 6 is comparative example 6 merely through the thick of hydrofluoric acid-ammonium fluoride buffer processing single-crystal strontium titanate substrate base surface
Rugosity analysis chart.
Fig. 7 is comparative example 6 merely through the three of hydrofluoric acid-ammonium fluoride buffer processing single-crystal strontium titanate substrate base surface
Tie up shape appearance figure.
Fig. 8 is according to embodiments of the present invention 1 by hydrofluoric acid-ammonium fluoride buffer and high temperature oxygen annealing while processing
The two-dimensional appearance figure on single-crystal strontium titanate substrate base surface.
Fig. 9 is according to embodiments of the present invention 1 by hydrofluoric acid-ammonium fluoride buffer and high temperature oxygen annealing while processing
The Roughness analysis figure on single-crystal strontium titanate substrate base surface.
Figure 10 is that according to embodiments of the present invention 1 process hydrofluoric acid-ammonium fluoride buffer and high temperature oxygen are annealed while being handled
Single-crystal strontium titanate substrate base surface three-dimensional appearance figure.
Specific embodiment
With reference to the accompanying drawing, specific embodiments of the present invention will be described in detail, it is to be understood that guarantor of the invention
Shield range is not limited by the specific implementation.
Unless otherwise explicitly stated, otherwise in entire disclosure and claims, term " includes " or its change
Changing such as "comprising" or " including " etc. will be understood to comprise stated element or component, and not exclude other members
Part or other component parts.
Strontium titanates substrate surface without any processing is relatively smooth, and surface undulation is smaller, basic no significant defect
Hole, surface Root Mean Square roughness are about 0.2nm (referring specifically to attached drawing 2-4).
Embodiment 1: the preparation method of the single-crystal strontium titanate substrate base with atom level step structure
Step includes:
(1) untreated strontium titanates substrate base is subjected to first time ultrasonic cleaning；The first time ultrasonic cleaning
Including three steps, cleaning step is successively: firstly, by untreated strontium titanates substrate base in acetone soln ultrasonic wave into
Row cleaning, the acetone soln ultrasonic cleaning time is 10min；Then, the strontium titanates substrate base after acetone soln being cleaned is in second
Ultrasonic wave is cleaned in alcoholic solution, and the ethanol solution ultrasonic cleaning time is 10min；Finally, the titanium after ethanol solution is cleaned
Sour strontium substrate base carries out ultrasonic cleaning in deionized water, and the deionized water ultrasonic cleaning time is 10min；
(2) the strontium titanates substrate base after the ammonium fluoride for being 5.0 with pH value-buffered hydrofluoric acid solution corrosion is cleaned for the first time,
Etching time is 40s；Then, the strontium titanates substrate base after buffering corrosion is subjected to ultrasonic cleaning 10min with deionized water；
(3) gained strontium titanates substrate base is made annealing treatment under temperature flowing oxygen atmosphere, the condition of annealing
It is: strontium titanates substrate base is placed in vacuum environment, be passed through the oxygen of flowing, control 1000 DEG C of temperature level, annealing time is
1h；
(4) the strontium titanates substrate base after annealing is subjected to second of ultrasonic cleaning, obtained with atom level platform
The single-crystal strontium titanate substrate base of stage structure；Second of ultrasonic cleaning includes three steps, is successively: firstly, by annealing
Strontium titanates substrate base after the reason ultrasonic wave in acetone soln is cleaned, and it is 10min that acetone soln, which is cleaned by ultrasonic the time,；So
Afterwards, strontium titanates substrate base after acetone soln the being cleaned ultrasonic wave in ethanol solution cleans, and ethanol solution ultrasound is clear
Washing the time is 10min；Finally, to carry out ultrasonic wave in deionized water clear for the strontium titanates substrate base after ethanol solution is cleaned
It washes, the deionized water ultrasonic cleaning time is 10min；And
(5) the single-crystal strontium titanate substrate base by resulting with atom level step structure carries out slice.
The result of gained single-crystal strontium titanate substrate base is referring to Fig. 8-10.By Fig. 8-10 it is found that, single-crystal strontium titanate substrate base
Piece surface is presented apparent step-like (0.35nm, 1 atom layer height of about strontium titanates), and entire ledge surface has no corruption
Borrosion hole hole occurs, and surface Root Mean Square roughness is about 0.13nm.Hand is handled compared to untreated and hydrofluoric acid-ammonium fluoride buffer
The substrate surface of section, this method processing shows desired step structure, and surface quality is very good, and it is thin to be conducive to high quality function
The growth of film.
Embodiment 2: the preparation method of the single-crystal strontium titanate substrate base with atom level step structure
Step includes:
(1) fluorination for being 4.5 by the strontium titanates substrate base pH value in embodiment 1 after first time ultrasonic cleaning
Strontium titanates substrate base after ammonium-buffered hydrofluoric acid solution corrosion cleaning for the first time, etching time is 45s；
(2) gained strontium titanates substrate base is made annealing treatment under temperature flowing oxygen atmosphere, the condition of annealing
It is: strontium titanates substrate base is placed in vacuum environment, be passed through the oxygen of flowing, controlled at 950 DEG C, annealing time is
1h；
(3) the strontium titanates substrate base after annealing is subjected to second of ultrasonic cleaning, cleaning method and step with
Embodiment 1 is identical；And
(4) the single-crystal strontium titanate substrate base by resulting with atom level step structure carries out slice.
Embodiment 3: the preparation method of the single-crystal strontium titanate substrate base with atom level step structure
Step includes:
(1) fluorination for being 5.5 by the strontium titanates substrate base pH value in embodiment 1 after first time ultrasonic cleaning
Strontium titanates substrate base after ammonium-buffered hydrofluoric acid solution corrosion cleaning for the first time, etching time is 35s；Then, by buffer corruption
Strontium titanates substrate base after erosion carries out ultrasonic cleaning 10min with deionized water；
(2) gained strontium titanates substrate base is made annealing treatment under temperature flowing oxygen atmosphere, the condition of annealing
It is: strontium titanates substrate base is placed in vacuum environment, be passed through the oxygen of flowing, controlled at 1100 DEG C, annealing time is
1h；
(3) the strontium titanates substrate base after annealing is subjected to second of ultrasonic cleaning, cleaning method and step with
Embodiment 1 is identical；And
(4) the single-crystal strontium titanate substrate base by resulting with atom level step structure carries out slice.
Comparative example 1:
The preparation method of single-crystal strontium titanate substrate base with atom level step structure, the difference with embodiment 1 is only
It is that ammonium fluoride-buffered hydrofluoric acid solution pH value is 4.0 (lower than 4.5).
The surface of gained single-crystal strontium titanate substrate also will appear ledge surface, but also will appear dell in step, high temperature oxygen
Annealing can not also eliminate step dell.
Comparative example 2:
The preparation method of single-crystal strontium titanate substrate base with atom level step structure, the difference with embodiment 2 is only
It is that etching time is 30s.
The surface of gained single-crystal strontium titanate substrate also will appear smooth step-like, but be the platform of half atom layer height
It is not thorough enough to illustrate that strontium-oxygen terminates surface corrosion, has a small amount of strontium-oxygen and the simultaneous surface of titanium-oxygen for rank.
Comparative example 3:
The preparation method of single-crystal strontium titanate substrate base with atom level step structure, the difference with embodiment 1 is only
It is that ammonium fluoride-buffered hydrofluoric acid solution pH value is 5.6.
The surface of gained single-crystal strontium titanate substrate also will appear ledge surface, but be half atom high step.
Comparative example 4:
The preparation method of single-crystal strontium titanate substrate base with atom level step structure, the difference with embodiment 2 is only
It is that ammonium fluoride-buffered hydrofluoric acid solution etching time is 29s (lower than 30s).
The surface of gained single-crystal strontium titanate substrate will not have any difference with preferential etching time.
Comparative example 5:
The preparation method of single-crystal strontium titanate substrate base with atom level step structure, the difference with embodiment 2 is only
It is that ammonium fluoride-buffered hydrofluoric acid solution etching time is 46s (being greater than 45s).
The surface of gained single-crystal strontium titanate substrate also will appear atom level ledge surface, but at step edge and step center
Locate defective hole, high temperature oxygen annealing is also difficult to eliminate.
Comparative example 6:
The preparation method of single-crystal strontium titanate substrate base with atom level step structure, the difference with embodiment 1 exist
In: hydrofluoric acid-ammonium fluoride buffer processing is only carried out, without annealing.
The result of gained single-crystal strontium titanate substrate base is referring to Fig. 5-7.By Fig. 5-7 it is found that being buffered through hydrofluoric acid-ammonium fluoride
The strontium titanates substrate surface still smoother of liquid processing, surface have that step-like (1 atom layer height of strontium titanates is about
0.39nm), laciniation is showed at step edge, and hole occurs at step center, overall surface rises and falls smaller still
Old to be no more than 0.2nm, basic no significant defect hole, surface Root Mean Square roughness is about 0.16nm.
The aforementioned description to specific exemplary embodiment of the invention is in order to illustrate and illustration purpose.These descriptions
It is not wishing to limit the invention to disclosed precise forms, and it will be apparent that according to the above instruction, can much be changed
And variation.The purpose of selecting and describing the exemplary embodiment is that explaining specific principle of the invention and its actually answering
With so that those skilled in the art can be realized and utilize a variety of different exemplary implementation schemes of the invention and
Various chooses and changes.The scope of the present invention is intended to be limited by claims and its equivalents.
Claims (10)
1. a kind of preparation method of the single-crystal strontium titanate substrate base with atom level step structure, which is characterized in that the preparation
Method includes:
(1) untreated strontium titanates substrate base is subjected to first time ultrasonic cleaning；
(2) the strontium titanates substrate base after being cleaned for the first time with ammonium fluoride-buffered hydrofluoric acid solution corrosion；
(3) strontium titanates substrate base obtained by step (2) is made annealing treatment under temperature flowing oxygen atmosphere；
(4) the strontium titanates substrate base after annealing is subjected to second of ultrasonic cleaning, obtained with atom level Step-edge Junction
The single-crystal strontium titanate substrate base of structure；And
(5) the resulting single-crystal strontium titanate substrate base with atom level step structure of step (4) is subjected to slice.
2. preparation method according to claim 1, which is characterized in that in step (1), the first time ultrasonic cleaning packet
Three steps are included, the cleaning step is successively: firstly, by untreated strontium titanates substrate base ultrasonic wave in acetone soln
It is cleaned, the acetone soln ultrasonic cleaning time is 5~30min；Then, the strontium titanates substrate base after acetone soln being cleaned
Ultrasonic wave is cleaned in ethanol solution, and the ethanol solution ultrasonic cleaning time is 5~30min；Finally, ethanol solution is cleaned
Strontium titanates substrate base afterwards carries out ultrasonic cleaning in deionized water, and the deionized water ultrasonic cleaning time is 5~30min.
3. preparation method according to claim 1, which is characterized in that in step (2), the ammonium fluoride-hydrofluoric acid buffering
The pH value of liquid is 4.5~5.5.
4. preparation method according to claim 3, which is characterized in that the preparation side of the ammonium fluoride-buffered hydrofluoric acid solution
Method is: by ammonium hydroxide (NH3-H2O it) carries out soda acid mixed configuration with HF to form, or by ammonium fluoride (NH4F it) is formed with HF mixed configuration.
5. preparation method according to claim 1, which is characterized in that in step (2), ammonium fluoride-buffered hydrofluoric acid solution
Etching time is 30~45s.
6. preparation method according to claim 1, which is characterized in that in step (3), the condition of the annealing is:
Strontium titanates substrate base is placed in vacuum environment, the oxygen of flowing is passed through, controls temperature within the scope of 950 DEG C~1100 DEG C,
Annealing time is 0.5~2h.
7. preparation method according to claim 1, which is characterized in that may further comprise: the titanium after buffering corrosion
Sour strontium substrate base is made annealing treatment again after being cleaned by ultrasonic with deionized water.
8. preparation method according to claim 7, which is characterized in that the time of deionized water ultrasonic cleaning is 5~
30min。
9. preparation method according to claim 1, which is characterized in that in step (4), second of ultrasonic cleaning packet
Three steps are included, the cleaning step is successively: firstly, the strontium titanates substrate base after annealing is surpassed in acetone soln
Sound wave is cleaned, and the acetone soln ultrasonic cleaning time is 5~30min；Then, the strontium titanates substrate after acetone soln being cleaned
Substrate ultrasonic wave in ethanol solution is cleaned, and the ethanol solution ultrasonic cleaning time is 5~30min；Finally, by ethanol solution
Strontium titanates substrate base after cleaning carries out ultrasonic cleaning in deionized water, and the deionized water ultrasonic cleaning time is 5~
30min。
10. the described in any item preparation methods of the claim 1-9 single-crystal strontium titanate obtained with atom level step structure serves as a contrast
Bottom substrate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910644631.XA CN110257912A (en) | 2019-07-17 | 2019-07-17 | Single-crystal strontium titanate substrate base and preparation method thereof with atom level step structure |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910644631.XA CN110257912A (en) | 2019-07-17 | 2019-07-17 | Single-crystal strontium titanate substrate base and preparation method thereof with atom level step structure |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110257912A true CN110257912A (en) | 2019-09-20 |
Family
ID=67926644
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910644631.XA Pending CN110257912A (en) | 2019-07-17 | 2019-07-17 | Single-crystal strontium titanate substrate base and preparation method thereof with atom level step structure |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110257912A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112176415A (en) * | 2020-09-23 | 2021-01-05 | 北京大学 | Method for obtaining single titanium oxide terminated insulating strontium titanate (001) surface |
| CN114000190A (en) * | 2021-10-28 | 2022-02-01 | 西湖大学 | Method for realizing high-flux film growth by adopting temperature gradient |
| CN114907116A (en) * | 2022-05-10 | 2022-08-16 | 武汉理工大学 | Preparation method of strontium titanate film with adjustable heat conductivity coefficient |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106784189A (en) * | 2016-12-26 | 2017-05-31 | 盐城工学院 | The preparation method of monocrystalline gallium oxide substrate base surface atom level ledge structure |
-
2019
- 2019-07-17 CN CN201910644631.XA patent/CN110257912A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106784189A (en) * | 2016-12-26 | 2017-05-31 | 盐城工学院 | The preparation method of monocrystalline gallium oxide substrate base surface atom level ledge structure |
Non-Patent Citations (2)
| Title |
|---|
| A. BISWAS, ET AL.,: ""Universal Ti-rich termination of atomically flat SrTiO3 (001), (110), and (111) surfaces"", 《APPLIED PHYSICS LETTERS》 * |
| 张竺立等: ""钛酸锶衬底表面改性对ＹＢＣＯ高温超导薄膜性能的影响"", 《低温物理学报》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112176415A (en) * | 2020-09-23 | 2021-01-05 | 北京大学 | Method for obtaining single titanium oxide terminated insulating strontium titanate (001) surface |
| CN114000190A (en) * | 2021-10-28 | 2022-02-01 | 西湖大学 | Method for realizing high-flux film growth by adopting temperature gradient |
| CN114000190B (en) * | 2021-10-28 | 2023-02-17 | 西湖大学 | Method for realizing high-flux film growth by adopting temperature gradient |
| CN114907116A (en) * | 2022-05-10 | 2022-08-16 | 武汉理工大学 | Preparation method of strontium titanate film with adjustable heat conductivity coefficient |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110257912A (en) | Single-crystal strontium titanate substrate base and preparation method thereof with atom level step structure | |
| CN104947192B (en) | A kind of Ca-Ti ore type SrIrO3The preparation method of monocrystal thin films material | |
| JP6886042B2 (en) | Formulation for selectively etching silicon germanium against silicon | |
| US6475860B2 (en) | Method for manufacturing a ferroelectric random access memory device | |
| Ramesh et al. | Scaling of ferroelectric properties in La‐Sr‐Co‐O/Pb‐La‐Zr‐Ti‐O/La‐Sr‐Co‐O capacitors | |
| JP2852355B2 (en) | Fine processing surface treatment agent | |
| CN105449045A (en) | Surface micro corrosion cleaning method applicable for crystal silicon wafer after RIE (Reactive Ion Etching) texturing | |
| US7008801B2 (en) | Method of forming ferroelectric thin films on a high-k layer | |
| CN107393818A (en) | A kind of secondary etching method of the soda acid of polysilicon solar cell and its polysilicon | |
| CN104393094B (en) | N-type silicon chip cleaning texturing method for HIT battery | |
| CN111763478B (en) | Chemical polishing solution for KDP crystal, preparation method and polishing method | |
| JP3095944B2 (en) | Method for producing oxide crystal thin film and thin film element | |
| CN112768348A (en) | Optimization method for etching lithium niobate material and improving side wall angle | |
| CN101613885B (en) | ZnGeP2 crystal corrosive and corrosion method | |
| Hirano et al. | Damage-Free Ultradiluted HF∕ Nitrogen Jet Spray Cleaning for Particle Removal with Minimal Silicon and Oxide Loss | |
| CN103872243A (en) | Method for manufacturing magnetic tunnel junction based on magnesium oxide target | |
| US7129184B2 (en) | Method of depositing an epitaxial layer of SiGe subsequent to a plasma etch | |
| KR20080103460A (en) | Metal substrate for a superconducting thin-film strip conductor | |
| JP3252052B2 (en) | Single crystal surface treatment method | |
| JP2000286396A (en) | Ferroelectric memory and manufacture thereof | |
| JP2880415B2 (en) | Non-mirror silicon wafer and method of manufacturing the same | |
| CN113026002A (en) | Thin film metal oxide structure and manufacturing method thereof | |
| CN118102860B (en) | Method for preparing bottom electrode of resistive random access memory based on in-situ growth method and application thereof | |
| JP2005156194A (en) | Capacitance temperature sensor | |
| JPS6293950A (en) | Manufacture of wafer |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20190920 |
|
| WD01 | Invention patent application deemed withdrawn after publication |