CN105679647B - The preparation method of substrate with atomically flating surface - Google Patents
The preparation method of substrate with atomically flating surface Download PDFInfo
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- CN105679647B CN105679647B CN201511014841.9A CN201511014841A CN105679647B CN 105679647 B CN105679647 B CN 105679647B CN 201511014841 A CN201511014841 A CN 201511014841A CN 105679647 B CN105679647 B CN 105679647B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
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Abstract
The present invention relates to a kind of preparation method of the substrate with atomically flating surface, this method includes the following steps：At least two pre-processed substrates of identical material are provided, each pre-processed substrate has an at least burnishing surface；At least two pre-processed substrate is stacked to form a laminate structure, wherein, the burnishing surfaces of adjacent two pre-processed substrates is opposite and completely overlapped setting；The laminate structure is placed on after being made annealing treatment in high temperature furnace, detaches the laminate structure.
Description
Technical field
Art of epitaxial growth more particularly to a kind of system of the substrate with atomically flating surface the present invention relates to film
Preparation Method.
Background technology
The substrate in thin film epitaxial growth field, for example, described in Chinese patent CN103184513A for growing high temperature
The SrTiO of superconducting thin film3Substrate is higher to the flatness requirement of substrate surface.In order to obtain the epitaxial growth film of high quality,
The prior art can in advance be handled the surface of substrate.For example, processing perovskite substrate (such as strontium titanates SrTiO3,
NdGaO3) and sodium chloride substrate (such as MgO) common method be by after substrate pre-wash (for example, substrate is placed on third
It is ultrasonically treated in ketone, isopropanol and ultra-pure water), some substrates such as SrTiO3, it is necessary to it impregnates to obtain by hot bath and diluted acid
Pre-processed substrate is placed in high-temperature annealing furnace by pre-processed substrate later, and high temperature is raised under gas oxygen atmosphere protection
It 1100 DEG C, stops about 3 hours and anneals, the migration of pre-processed substrate surface atom is made to improve the flatness of substrate surface.But in reality
In, the impurity that substrate itself has easily is precipitated in annealing process and generates non-single terminal surface for pre-processed substrate.Example
Such as, when using existing method preparation SrTiO3During substrate, the SrTiO of acquisition3Substrate can form a large amount of strontium oxide strontias (SrO) terminal surface
With titanium oxide (TiO2) terminal surface mixes, the titanium oxide (TiO single without forming large area2) terminal surface, because of film growth pair
Terminal surface is sensitive, and certain surfaces will be unable to realize epitaxial growth, cause film quality inhomogenous.
Invention content
In view of this, it is necessory to provide it is a kind of it is simple for process, be easily achieved, controllability is good has atomically flating table
The preparation method of the substrate in face.
A kind of preparation method of the substrate with atomically flating surface, this method include the following steps：Identical material is provided
At least two pre-processed substrates of material, each pre-processed substrate have an at least burnishing surface；By described at least two pre- places
Reason substrate is stacked to form a laminate structure, wherein, the burnishing surface of adjacent two pre-processed substrates is opposite
And completely overlapped setting；The laminate structure is placed on after being made annealing treatment in high temperature furnace, detaches the stepped construction
Body.
Relative to the prior art, the preparation method of the substrate provided by the invention with atomically flating surface is with following
Advantageous effect：By the burnishing surface of at least two adjacent pre-processed substrates is opposite and completely overlapped setting, a stepped construction is formed
Body, and the laminate structure is placed in high temperature furnace and is made annealing treatment, due to the polishing of two adjacent pre-processed substrates
Because of completely overlapped and contact setting, adjacent two burnishing surfaces fit together almost in contact with less than gas, make a pre- place in face
It is the body phase of pre-processed substrate adjacent thereto on the outside of the burnishing surface of reason substrate, and then each substance group in the interior outside of burnishing surface
Part gradient difference no longer exist, body phase substance is suppressed to the migration at burnishing surface, also may refrain from substance to gaseous evaporation,
The precipitation of itself impurity on burnishing surface can be prevented, and single terminal surface can be formed in burnishing surface.In addition, due to adjacent
The burnishing surface of two pre-processed substrates is completely overlapped in annealing process and contact is set, so as to reduce impurity particle in atmosphere
Pollution to burnishing surface.The preparation method of substrate provided by the invention with atomically flating surface is simple for process, it is real to be easy to
Existing and controllability is good.
Description of the drawings
Fig. 1 is the flow chart of the preparation method of the substrate provided in an embodiment of the present invention with atomically flating surface.
Fig. 2 is the SrTiO that the embodiment of the present invention 1 has atomically flating surface3Treated for substrate and comparative example 1
SrTiO3The comparison diagram of (001) surface reflection high energy electron spectrum (RHEED) figure of substrate.
Fig. 3 is the SrTiO that the embodiment of the present invention 1 has atomically flating surface3The atomic force microscope (AFM) of substrate
Figure.
Fig. 4 is treated the SrTiO of comparative example 13The AFM figures of substrate.
Fig. 5 is the AFM figures for the MgO substrates that the embodiment of the present invention 2 has atomically flating surface.
Fig. 6 is the AFM figures of treated the MgO substrates of comparative example 2.
Fig. 7 is the NdGaO that the embodiment of the present invention 3 has atomically flating surface3The AFM figures of substrate.
Following specific embodiment will be further illustrated the present invention with reference to above-mentioned attached drawing.
Specific embodiment
Below in conjunction with the accompanying drawings and the specific embodiments, the preparation of the substrate with atomically flating surface is provided the present invention
Method is described in further detail.
Referring to Fig. 1, an embodiment of the present invention provides a kind of preparation method of the substrate with atomically flating surface, it should
Method includes the following steps：
S10 provides two pre-processed substrates of identical material, and each pre-processed substrate has an at least burnishing surface；
Two pre-processed substrates are stacked to form a laminate structure by S20, wherein, two pretreatment linings
The burnishing surface at bottom is opposite and completely overlapped setting；
The laminate structure is placed on after being made annealing treatment in high temperature furnace, detaches the laminate structure by S30,
Obtain two substrates with atomically flating surface.
In the step S10, each pre-processed substrate has an at least burnishing surface, and the burnishing surface is the pre- place
Reason substrate is used to form the surface of atomically flating.The burnishing surface be a smooth surface, the surface roughness of the burnishing surface
Maximum can be tens nanometers.Preferably, the surface roughness of the burnishing surface can be 0.5nm~1.5nm, have the roughness
The burnishing surface, advantageously form atomically flating surface.As long as ensure two pre-processed substrates adjacent in S20
The burnishing surface completely overlapped can be set, i.e., the shape and area of the burnishing surface of adjacent two pre-processed substrates
Corresponding, the shape of the substrate is unlimited, can select according to actual needs.In the present embodiment, the rough surface of the burnishing surface
It spends for 0.5nm~1.5nm.The substrate is cuboid, and the burnishing surface is rectangle.
The pre-processed substrate can be nonreactive with water and need to form the thin film epitaxy with atomically flating surface
Growth substrate.For example, the pre-processed substrate can be perovskite substrate and sodium chloride substrate.Wherein, the perovskite
Class substrate can be strontium titanates (SrTiO3) substrate, gallic acid neodymium (NdGaO3) substrate, calcium titanate (CaTiO3) substrate or lanthanum aluminate
(LaAlO3) substrate.The sodium chloride substrate can be magnesia (MgO) substrate.
In one embodiment, can further comprise cleaning initial substrate to obtain the pretreatment in the step S10
The step of substrate.Specifically, common method of the prior art can be used to clean initial substrate, for example, can be by described in
Initial substrate be placed sequentially in acetone, isopropanol, pure water container in supersound process progress is carried out to the initial substrate
Cleaning.
In another embodiment, for certain materials, particularly perovskite (ABO3) initial substrate, can further wrap
The step of hot bath and/or diluted acid immersion are carried out to the initial substrate after the cleaning is included, to obtain in the step S10
The pre-processed substrate.In this step, hot water can remove the AO water with the hydrate that AO layers of reaction bonded are AO, diluted acid
Object is closed, is left BO2Layer is used to form atomically flating surface.Specifically, when the perovskite substrate is SrTiO3During substrate,
It can be by the SrTiO after cleaning3Substrate is pre-processed by hot bath and diluted acid immersion, removes SrTiO3Substrate surface can
Strontium oxide strontia (SrO) layer reacted with diluted acid is left titanium oxide (TiO2) layer is used to form atomically flating surface.The hot water
Temperature is on 90 DEG C~100 DEG C.The diluted acid can be the common diluted acid for impregnating the initial substrate in the prior art, e.g., dilute
Hydrochloric acid, hydrofluoric acid etc..A concentration of the 5%~37% of the diluted acid.In the present embodiment, using described in a concentration of 10% salt acid soak
Initial substrate.
In the step S20, two pre-processed substrates can be stacked to form the stacking knot in the following manner
Structure body：
Two pre-processed substrates are totally submerged in a solvent by S21；And
S22, by the burnishing surface of two pre-processed substrates in the solvent opposite and completely overlapped setting, shape
Into the laminate structure.
In the step S21, the solvent for purity it is high, can evaporate in subsequent annealing process and not with the pre- place
Manage the solvent of substrate reaction.The purity of the solvent is 99.9%~99.999%.In the present embodiment, the solvent is pure water.
The purity of the pure water can be represented with resistance value, it is preferable that the resistance value of the pure water is 18.3 mega-ohm centimeters (M Ω
Cm more than).
In the step S21, as long as two pre-processed substrates can be made to be fully immersed in the solvent, example
Such as, two pre-processed substrates can be placed in the container equipped with the solvent.Preferably, by two pretreatments
After substrate is immersed in the solvent, it can further comprise the step of the burnishing surface of two pre-processed substrates of a cleaning
Suddenly.The burnishing surface of the pre-processed substrate can adhere to a small amount of impurity, the cleaning in air before solvent is placed on
Step can make a small amount of impurity for being attached to the burnishing surface come off in a solvent, reduce by two throwings of completely overlapped setting
Impurity between smooth surface, conducive to the atomically flating surface of high quality is formed.The cleaning step can clean institute by ultrasonic vibration
State burnishing surface.
In the step S23, if can guarantee the burnishing surfaces of two pre-processed substrates it is opposite in a solvent and
Completely overlapped setting, the laminating method of two pre-processed substrates are unlimited.For example, clamping device can be passed through in the solvent
One pre-processed substrate is attached to the completely overlapped setting that the burnishing surface is realized in another described pre-processed substrate manually；
It is completely heavy close to realizing that the methods of electric sucking disc can also be used makes the burnishing surface of two pre-processed substrates attract each other
Folded setting.There is a solvent membrane formed by the solvent, the solvent between the burnishing surface of two pre-processed substrates
Film is in close contact setting with two opposite burnishing surfaces, can exclude the air between two opposite burnishing surfaces, and
The atmosphere in external environment can be completely cut off simultaneously between two opposite burnishing surfaces.
In the present embodiment, a pre-processed substrate is attached to manually by another described pretreatment by clamping device and is served as a contrast
The completely overlapped setting of the burnishing surface is realized on bottom, has one between the burnishing surface of adjacent two pre-processed substrates
Pure water film.
In another embodiment, other methods can also be used to be formed between the burnishing surface of two pre-processed substrates
One solvent membrane.For example, it can coat or spray described molten in the whole surface of the burnishing surface of a pre-processed substrate
Then another described pre-processed substrate is layered in the pre-processed substrate of sprinkling solvent, the solvent is made to be clipped in two by agent
Between the burnishing surface, and the burnishing surface of two pre-processed substrates is in close contact setting with the solvent；Or
It is taken out after one pre-processed substrate is immersed in the solvent, solvent is made to be attached to the whole surface of the burnishing surface, then
Another described pre-processed substrate is layered on the solvent, make the burnishing surfaces of two pre-processed substrates with it is described
Solvent is in close contact setting.
Further, two pre-processed substrates also can be stacked to form the laminate structure in the following manner：
S21 ' cleans the burnishing surface of two pre-processed substrates；
Two pre-processed substrates are directly fitted, form the laminate structure by S22 ' in dry conditions.
In the step S21 ', specifically, the burnishing surface that gas purges the pre-processed substrate can be used, make described
The impurity adhered on burnishing surface is detached from the burnishing surface with the purging of gas, to improve the cleanliness factor of the burnishing surface, can subtract
It is completely overlapped and directly fit the impurity between the burnishing surface of two together in few step S22 '.For example, it can adopt
The burnishing surface of the pre-processed substrate is purged with nitrogen gun.
In the step S22 ', as long as can guarantee the burnishing surface of two adjacent pre-processed substrates in dried strip
Opposite and completely overlapped setting, the laminating method of two pre-processed substrates are unlimited under part.The drying condition is preferably thousand
Grade ultra-clean chamber and more excellent environment.Since the burnishing surface smoothness is higher, two adjacent pre-processed substrates it is described
Burnishing surface is completely overlapped in dry conditions and when directly fitting, can exclude most of sky between two opposite burnishing surfaces
Gas, and most of atmosphere in external environment can be completely cut off simultaneously between two opposite burnishing surfaces.
In the step S30, the laminate structure is placed on when being made annealing treatment in high temperature furnace, it can be in annealing atmosphere
It anneals 2-4 hours under certain annealing temperature under enclosing, the surface with atomically flating is formed in the burnishing surface.Then, will
The laminate structure separation, obtains two substrates with atomically flating surface.The annealing atmosphere can be according to practical need
It is selected, can be oxygen, Ar gas, nitrogen or normal atmospheric atmosphere.The annealing temperature can be selected according to substrate,
It can be 400 DEG C~1200 DEG C.In the present embodiment, the annealing atmosphere is oxygen.The annealing temperature is 1000 DEG C -1100 DEG C.
In annealing process, although two burnishing surfaces can inevitably make air when directly fitting in dry conditions
In pollutant or surface adsorbate be mixed between two burnishing surfaces, but relative in the prior art by pre-processed substrate
It is directly exposed to high temperature stove fire to be made annealing treatment, since the burnishing surface of two pre-processed substrates is in annealing process
Completely overlapped and contact setting, greatly reduces pollution of the impurity particle to the burnishing surface in annealing atmosphere；In addition, two pre-
The burnishing surface of substrate is handled because completely overlapped and contact setting, the burnishing surface fit together almost in contact with less than annealing
Gas in stove, make be on the outside of the burnishing surface of a pre-processed substrate another pre-processed substrate body
Phase, and then the gradient difference of the substance component in outside no longer exists in each burnishing surface, body phase substance is at the burnishing surface
Migration be suppressed, also may refrain from substance to gaseous evaporation, the precipitation of itself impurity on the burnishing surface can be prevented, and
And single terminal surface can be formed in the burnishing surface.
When the burnishing surface completely overlapped setting in a solvent of two pre-processed substrates, two pretreatments
There is one layer of solvent membrane between the burnishing surface of substrate, which evaporates in annealing process with the raising of temperature,
The burnishing surface of two pre-processed substrates can be made closely to fit together, so as to avoid impurity in annealing atmosphere
Pollution of the particle to the burnishing surface, avoids and pre-processed substrate is directly exposed in high temperature stove fire the institute that anneals in the prior art
Caused by pollution to pre-processed substrate surface；In addition, two burnishing surfaces being closely bonded are not exposed to gas, make
It is the body phase of another pre-processed substrate on the outside of the burnishing surface of one pre-processed substrate, and then each described
The gradient difference of the substance component in outside no longer exists in burnishing surface, and body phase substance is suppressed to the migration at the burnishing surface,
Substance may refrain to gaseous evaporation, the precipitation of itself impurity on the burnishing surface can have been prevented, and in the burnishing surface
Single terminal surface can be formed.
Further, the quantity for being stacked the pre-processed substrate is not limited to two, as long as ensuring the adjacent pre- place
Manage substrate the burnishing surface is opposite and completely overlapped setting, the quantity of the pre-processed substrate can be multiple.
Embodiment 1
Two SrTiO with burnishing surface are provided3Substrate is placed sequentially in each ultrasonic five in acetone, isopropanol, ultra-pure water
After minute is cleaned, by SrTiO3After substrate hot bath is impregnated 1 hour, it is placed in a concentration of 10% hot hydrochloric acid (HCl)
It impregnates 45 minutes, obtains two SrTiO3Pre-processed substrate.By two SrTiO3Pre-processed substrate is laminated in pure water, makes two
SrTiO3The burnishing surface of pre-processed substrate is opposite and overlaps, and obtains a laminate structure.Above-mentioned laminate structure is placed
It in high temperature furnace, after annealing 3 hours at a temperature of 1080 DEG C under oxygen atmosphere, is detached, obtaining two has atom level
The SrTiO of flat surface3Substrate.
Comparative example 1
One SrTiO with burnishing surface is provided3Substrate is placed sequentially in each ultrasonic five in acetone, isopropanol, ultra-pure water
After minute is cleaned, by SrTiO3After substrate is placed on hot bath immersion 1 hour, it is placed in a concentration of 10% hot hydrochloric acid
It impregnates 45 minutes, obtains a SrTiO3Pre-processed substrate.By above-mentioned SrTiO3Pre-processed substrate is placed in high temperature furnace, in oxygen
After atmosphere is annealed 3 hours at a temperature of enclosing lower 1080 DEG C, a treated SrTiO is obtained3Substrate.
Fig. 2 is referred to, Fig. 2 (a) is the SrTiO with atomically flating surface that this case embodiment 1 obtains3Substrate
(001) reflection high energy electron spectrum (RHEED) figure on surface, Fig. 2 (b) is treated the SrTiO of comparative example 13(001) table of substrate
Reflection high energy electron spectrum (RHEED) figure in face, comparison diagram 2 (a) and Fig. 2 (b) are as can be seen that the acquisition of this case embodiment 1 has
The SrTiO on atomically flating surface3(001) surface of substrate is relative to treated the SrTiO of comparative example 13(001) table of substrate
It is face clear-cut texture, sharp, illustrate the SrTiO with atomically flating surface that this case embodiment 1 obtains3(001) table of substrate
The periodicity of face atomic arrangement is good, and surface has atomically flating.
Refer to Fig. 3 and Fig. 4, it can be seen that the SrTiO with atomically flating surface that this case embodiment 1 obtains3Lining
The surface at bottom forms single terminal surface；Comparative example 1 obtains treated SrTiO3Substrate surface generates step structure, and
Double terminal surfaces are formed at step.
Embodiment 2
Two MgO substrates with burnishing surface are provided, are placed sequentially in acetone, isopropanol, ultra-pure water each ultrasonic five points
After clock is cleaned, two MgO pre-processed substrates are obtained.Two MgO pretreatments in pure water are laminated, two MgO is made to locate in advance
The burnishing surface relative superposition setting of substrate is managed, obtains a laminate structure.Above-mentioned laminate structure is placed in high temperature furnace,
It after annealing 3 hours at a temperature of lower 1080 DEG C of oxygen atmosphere, is detached, obtains two MgO with atomically flating surface
Substrate.
Comparative example 2
One MgO substrate with burnishing surface is provided, is placed sequentially in acetone, isopropanol, ultra-pure water each ultrasonic five points
After clock is cleaned, a MgO pre-processed substrate is obtained.The MgO pre-processed substrates are placed in high temperature furnace, in oxygen atmosphere
Under anneal 3 hours at 1080 DEG C, obtain treated MgO substrates.
Refer to Fig. 5 and Fig. 6, it can be seen that the MgO substrates with atomically flating surface that this case embodiment 2 obtains
Surface cleaning free from admixture；A large amount of Ga impurity is precipitated in treated the MgO substrate surfaces of comparative example 1.
Embodiment 3
Two NdGaO with burnishing surface are provided3Substrate is placed sequentially in each ultrasonic five in acetone, isopropanol, ultra-pure water
After minute is cleaned, by NdGaO3After substrate hot bath is impregnated 1 hour, it is placed in a concentration of 10% hot hydrochloric acid (HCl)
It impregnates 45 minutes, obtains two NdGaO3Pre-processed substrate.By two NdGaO3Pre-processed substrate is laminated in pure water, makes two
NdGaO3The burnishing surface of pre-processed substrate is opposite and overlaps, and obtains a laminate structure.Above-mentioned laminate structure is placed
It in high temperature furnace, after annealing 3 hours at a temperature of 1080 DEG C under oxygen atmosphere, is detached, obtaining two has atom level
The NdGaO of flat surface3Substrate.
Refer to Fig. 7, the NdGaO with atomically flating surface that this case embodiment 3 obtains3The surface of substrate forms
Single terminal surface.
The preparation method of substrate provided by the invention has the advantages that：By at least two adjacent pre-processed substrates
Burnishing surface is opposite and completely overlapped setting, form a laminate structure, and by the laminate structure be placed in high temperature furnace into
Row annealing, since the burnishing surface of two adjacent pre-processed substrates is because of completely overlapped and contact setting, adjacent two throwings
Smooth surface fits together almost in contact with less than gas, and it is pre- place adjacent thereto on the outside of the burnishing surface of a pre-processed substrate to make
The body phase of substrate is managed, and then the gradient difference of the substance component in outside no longer exists in each burnishing surface, body phase substance is to burnishing surface
The migration at place is suppressed, and also may refrain from substance to gaseous evaporation, can have been prevented the precipitation of itself impurity on burnishing surface, and
Single terminal surface can be formed in burnishing surface.In addition, since the burnishing surface of two adjacent pre-processed substrates is in annealing process
Completely overlapped and contact setting, so as to reduce pollution of the impurity particle to burnishing surface in atmosphere.It is provided by the invention that there is original
The preparation method of the substrate of sub- grade flat surface is simple for process, be easily achieved and controllability is good.
In addition, those skilled in the art can also do other variations in spirit of the invention, certainly, these are smart according to the present invention
The variation that god is done should all include within scope of the present invention.
Claims (6)
1. a kind of preparation method of the substrate with atomically flating surface, this method include the following steps：
S10 provides at least two pre-processed substrates of identical material, and each pre-processed substrate has an at least burnishing surface；
At least two pre-processed substrate is impregnated in a solvent, makes the described of two adjacent pre-processed substrates by S20
Burnishing surface is opposite in the solvent and completely overlapped setting, forms a laminate structure；And
The laminate structure is placed on after being made annealing treatment in high temperature furnace, detaches the laminate structure by S30.
2. the preparation method of the substrate with atomically flating surface as described in claim 1, which is characterized in that the polishing
The surface roughness in face is 0.5nm~1.5nm.
3. the preparation method of the substrate with atomically flating surface as described in claim 1, which is characterized in that the solvent
For pure water, more than the resistivity 18.3M Ω cm of the pure water.
4. the preparation method of the substrate with atomically flating surface as described in claim 1, which is characterized in that adjacent two
There is a pure water film, the pure water film connects with two opposite burnishing surfaces between the burnishing surface of a pre-processed substrate
Touch setting.
5. the preparation method of the substrate with atomically flating surface stated such as claim 1, which is characterized in that the substrate is
Strontium titanates substrate, gallic acid neodymium substrate, calcium titanate substrate, lanthanum aluminate substrate or magnesia substrate.
6. the preparation method of the substrate with atomically flating surface as described in claim 1, which is characterized in that the stacking
Structure is annealed at a temperature of 1000 DEG C -1100 DEG C.
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| CN110265191A (en) * | 2019-06-14 | 2019-09-20 | 清华大学 | SrTiO3Polycrystalline circle substrate and preparation method thereof |
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| CN106702327B (en) * | 2017-01-10 | 2019-10-11 | 河北大学 | A kind of optimization method of ultra-thin lanthanum nickelate thin film electronic transport performance |
| CN110246957B (en) * | 2019-06-14 | 2022-04-15 | 清华大学 | Ultra-high vacuum processing of SrTiO3Method for preparing FeSe superconductive film and substrate |
| CN110512286A (en) * | 2019-08-26 | 2019-11-29 | 清华大学 | The method that exchange annealing prepares FeSe polycrystalline circle superconducting thin film |
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