CN105679647A - Preparation method for substrates with atomic-scale flat surfaces - Google Patents
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- CN105679647A CN105679647A CN201511014841.9A CN201511014841A CN105679647A CN 105679647 A CN105679647 A CN 105679647A CN 201511014841 A CN201511014841 A CN 201511014841A CN 105679647 A CN105679647 A CN 105679647A
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
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Abstract
The invention relates to a preparation method for substrates with atomic-scale flat surfaces. The preparation method comprises the following steps of providing at least two preprocessed substrates with the same material, wherein each preprocessed substrate is equipped with at least a polished surface; enabling the at least two preprocessed substrates to be laminated to form a laminated structural body, wherein the polished surfaces of the adjacent two preprocessed substrates are opposite and are fully overlapped; and putting the laminated structural body in a high-temperature furnace to be subjected to annealing treatment, and separating the laminated structural body.
Description
Technical field
The present invention relates to the art of epitaxial growth of thin film, the preparation method particularly relating to a kind of substrate with atomically flating surface.
Background technology
The substrate in thin film epitaxial growth field, for instance the SrTiO for growing high-temperature superconducting thin film recorded in Chinese patent CN103184513A3Substrate is higher to the flatness requirement of substrate surface. In order to obtain high-quality epitaxial growth film, the surface of substrate can be processed by prior art in advance. Such as, perovskite substrate is processed (such as strontium titanates SrTiO3, NdGaO3) and the common method of sodium chloride substrate (such as MgO) be after substrate is cleaned in advance (such as, substrate is placed on supersound process in acetone, isopropanol and ultra-pure water), some substrate such as SrTiO3Must pass through hot bath and diluted acid soaks to obtain pre-processed substrate, afterwards pre-processed substrate is placed in high-temperature annealing furnace, under gas oxygen atmosphere protection, is raised to high temperature 1100 DEG C; stop annealing in about 3 hours, make pre-processed substrate surface atom migrate the flatness improving substrate surface. But in actual applications, pre-processed substrate easily precipitates out impurity that substrate self has in annealing process and generates non-single terminal surface. Such as, when adopting existing method to prepare SrTiO3During substrate, it is thus achieved that SrTiO3Substrate can form a large amount of strontium oxide (SrO) terminal surface and titanium oxide (TiO2) terminal surface mixes, the titanium oxide (TiO single without forming large area2) terminal surface, because thin film growth is sensitive to terminal surface, some surface will be unable to realize epitaxial growth, causes film quality heterogeneity.
Summary of the invention
In view of this, a kind of technique of necessary offer is simple, be easily achieved, the preparation method of the substrate with atomically flating surface that controllability is good.
A kind of preparation method of the substrate with atomically flating surface, the method comprises the following steps: providing at least two pre-processed substrate of identical material, each described pre-processed substrate has at least one burnishing surface; Described at least two pre-processed substrate stacking arranges formation one laminate structure, and wherein, the described burnishing surface of two adjacent described pre-processed substrate is relative and completely overlapped setting; After being placed in high temperature furnace by described laminate structure to be annealed and processing, separate described laminate structure.
Relative to prior art, the preparation method of the substrate with atomically flating surface provided by the invention has the advantages that relative for the burnishing surface of adjacent at least two pre-processed substrate and completely overlapped setting, form a laminate structure, and this laminate structure is placed in high temperature furnace and is annealed process, owing to the burnishing surface of two adjacent pre-processed substrate is because of completely overlapped and contact setting, two adjacent burnishing surfaces fit together almost in contact with less than gas, making the outside of the burnishing surface of a pre-processed substrate is the body phase of pre-processed substrate adjacent thereto, and then the gradient difference of the material component in outside no longer exists in each burnishing surface, body phase material is suppressed to the migration at burnishing surface place, also may refrain from the material evaporation to gaseous state, the precipitation being possible to prevent on burnishing surface self impurity, and single terminal surface can be formed at burnishing surface. further, since the completely overlapped and contact setting in annealing process of the burnishing surface of adjacent two pre-processed substrate, thus decreasing the impurity particle pollution to burnishing surface in atmosphere. the preparation method technique of the substrate with atomically flating surface provided by the invention is simple, be easily achieved and controllability is good.
Accompanying drawing explanation
Fig. 1 is the flow chart of the preparation method of the substrate with atomically flating surface that the embodiment of the present invention provides.
Fig. 2 is the SrTiO that the embodiment of the present invention 1 has atomically flating surface3SrTiO after substrate and comparative example 1 process3The 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 surface3Atomic force microscope (AFM) figure of substrate.
Fig. 4 is the SrTiO after comparative example 1 processes3The AFM figure of substrate.
Fig. 5 is the AFM figure that the embodiment of the present invention 2 has the MgO substrate on atomically flating surface.
Fig. 6 is the AFM figure of the MgO substrate after comparative example 2 processes.
Fig. 7 is the NdGaO that the embodiment of the present invention 3 has atomically flating surface3The AFM figure of substrate.
Following detailed description of the invention will further illustrate the present invention in conjunction with above-mentioned accompanying drawing.
Detailed description of the invention
Below in conjunction with the accompanying drawings and the specific embodiments, the preparation method of the substrate with atomically flating surface is provided to be described in further detail the present invention.
Refer to Fig. 1, the preparation method embodiments providing a kind of substrate with atomically flating surface, the method comprises the following steps:
S10, it is provided that two pre-processed substrate of identical material, each described pre-processed substrate has at least one burnishing surface;
These two pre-processed substrate stackings are arranged formation one laminate structure by S20, and wherein, the described burnishing surface of two described pre-processed substrate is relative and completely overlapped setting;
S30, after being placed in high temperature furnace by described laminate structure to be annealed and processing, separates described laminate structure, it is thus achieved that two substrates with atomically flating surface.
In described step S10, each described pre-processed substrate has at least one burnishing surface, and described burnishing surface is that described pre-processed substrate is for forming the surface of atomically flating. Described burnishing surface is a smooth surface, and the surface roughness of described burnishing surface is maximum is tens nanometers. Preferably, the surface roughness of described burnishing surface can be 0.5nm ~ 1.5nm, has the described burnishing surface of described roughness, advantageously forms atomically flating surface. As long as ensureing that the described burnishing surface of two described pre-processed substrate adjacent in S20 can completely overlapped be arranged, shape and the area of the described burnishing surface of two namely adjacent described pre-processed substrate are corresponding, the shape of described substrate is not limit, and can select according to actual needs. In the present embodiment, the surface roughness of described burnishing surface is 0.5nm ~ 1.5nm. Described substrate is cuboid, and described burnishing surface is rectangle.
Described pre-processed substrate can be nonreactive with water and need to form the thin film epitaxial growth substrate with atomically flating surface. Such as, described pre-processed substrate can be perovskite substrate and sodium chloride substrate. Wherein, described perovskite substrate can be strontium titanates (SrTiO3) substrate, gallic acid neodymium (NdGaO3) substrate, calcium titanate (CaTiO3) substrate or lanthanum aluminate (LaAlO3) substrate. Described sodium chloride substrate can be magnesium oxide (MgO) substrate.
In one embodiment, can farther include to clean initial substrate to obtain the step of the described pre-processed substrate in described step S10. Specifically, can adopt common method of the prior art that initial substrate is carried out, for instance, can be sequentially placed in the container with acetone, isopropanol, pure water by described initial substrate described initial substrate is carried out supersound process and be carried out.
In another embodiment, for some material, particularly perovskite (ABO3) initial substrate, can farther include the described initial substrate after this cleaning is carried out hot bath and/or step that diluted acid soaks, to obtain the described pre-processed substrate in described step S10. In this step, hot water can be the hydrate of AO with AO layer reaction bonded, and diluted acid can remove this AO hydrate, remaining BO2Layer is used for forming atomically flating surface. Specifically, when described perovskite substrate is SrTiO3During substrate, can by the SrTiO after cleaning3Substrate is soaked by hot bath and diluted acid and carries out pretreatment, removes SrTiO3Strontium oxide (SrO) layer that can react with diluted acid of substrate surface, remaining titanium oxide (TiO2) layer is used for forming atomically flating surface. The temperature of described hot water is on 90 DEG C～100 DEG C. Described diluted acid can be the conventional diluted acid soaking described initial substrate in prior art, e.g., and dilute hydrochloric acid, Fluohydric acid. etc. The concentration of described diluted acid is 5% ~ 37%. In the present embodiment, adopting concentration is initial substrate described in 10% soak with hydrochloric acid.
In described step S20, two described pre-processed substrate stacking can arrange the described laminate structure of formation in the following manner:
Two described pre-processed substrate are totally submerged in a solvent by S21; And
S22, by the relative and completely overlapped setting in described solvent of the described burnishing surface of two described pre-processed substrate, forms described laminate structure.
In described step S21, the solvent that described solvent is that purity is high, can evaporate and do not react with described pre-processed substrate in follow-up annealing process. The purity of described solvent is 99.9%～99.999%. In the present embodiment, described solvent is pure water. The purity of described pure water can be represented, it is preferable that the resistance value of described pure water is more than 18.3 megaohms/centimetre (M Ω/cm) with resistance value.
In described step S21, as long as two described pre-processed substrate can be made to be fully immersed in described solvent, for instance, it is possible to two described pre-processed substrate are placed in the container equipped with described solvent. Preferably, after being immersed in described solvent by two described pre-processed substrate, the step of the described burnishing surface of two described pre-processed substrate of cleaning can be farther included. The described burnishing surface of described pre-processed substrate can adhere to a small amount of impurity in atmosphere before being placed on solvent, described cleaning step can make a small amount of impurity being attached to described burnishing surface come off in a solvent, reduce by the impurity between two described burnishing surfaces of completely overlapped setting, be beneficial to the high-quality atomically flating surface of formation. Described cleaning step can clean described burnishing surface by ultrasonic vibration.
In described step S23, as long as can guarantee that the described burnishing surface of two described pre-processed substrate is relative in a solvent and completely overlapped setting, the laminating method of two described pre-processed substrate is not limit. Such as, by clamping device, manually pre-processed substrate described in can be attached to the completely overlapped setting realizing described burnishing surface in another described pre-processed substrate in described solvent; May be used without the methods such as electric sucking disc makes the described burnishing surface of two described pre-processed substrate attract each other and realize completely overlapped setting. There is between the described burnishing surface of two described pre-processed substrate a solvent membrane formed by described solvent, described solvent membrane is all in close contact setting with relative two described burnishing surfaces, the air between the described burnishing surface of relative two can be got rid of, and can completely cut off between two described burnishing surfaces that the atmosphere entrance in external environment condition is relative simultaneously.
In the present embodiment, manually a described pre-processed substrate is attached to by clamping device the completely overlapped setting realizing described burnishing surface in another described pre-processed substrate, there is between the described burnishing surface of two adjacent described pre-processed substrate a pure water film.
In another embodiment, it is possible to adopt additive method to form solvent membrane described between the described burnishing surface of two described pre-processed substrate. Such as, can in the whole surface-coated of the described burnishing surface of pre-processed substrate described in one or spray described solvent, then another described pre-processed substrate is layered in the pre-processed substrate spraying solvent, make described solvent be clipped between two described burnishing surfaces, and the described burnishing surface of two described pre-processed substrate is all in close contact setting with described solvent; Or take out after pre-processed substrate described in is immersed in described solvent, solvent is made to be attached to the whole surface of described burnishing surface, then another described pre-processed substrate is layered on described solvent, makes the described burnishing surface of two described pre-processed substrate and described solvent all be in close contact setting.
Further, two described pre-processed substrate arrange the described laminate structure of formation also by the following manner stacking:
S21 ', the described burnishing surface of two described pre-processed substrate of cleaning;
Two described pre-processed substrate are directly fitted, are formed described laminate structure by S22 ' in dry conditions.
In described step S21 ', specifically, the described burnishing surface of pre-processed substrate described in gas purging can be adopted, the impurity adhered on described burnishing surface is made to depart from described burnishing surface along with the purging of gas, to improve the cleanliness factor of described burnishing surface, can reduce completely overlapped in described step S22 ' and directly against the impurity between the described burnishing surface of two be combined. Such as, nitrogen gun can be adopted to purge the described burnishing surface of described pre-processed substrate.
In described step S22 ', as long as can guarantee that the described burnishing surface of the described pre-processed substrate of adjacent two is relative in dry conditions and completely overlapped setting, the laminating method of two described pre-processed substrate is not limit. Described drying condition is preferably thousand grades of ultra-clean chambers and more excellent environment. Owing to described burnishing surface smoothness is higher, the described burnishing surface of two adjacent described pre-processed substrate is completely overlapped in dry conditions and when directly fitting, the most of air between the described burnishing surface of relative two can be got rid of, and can completely cut off between two described burnishing surfaces that the most of atmosphere entrance in external environment condition is relative simultaneously.
In described step S30, it is placed in high temperature furnace by described laminate structure to be annealed when processing, can anneal 2-4 hour under certain annealing temperature under annealing atmosphere, form the surface with atomically flating at described burnishing surface. Then, described laminate structure is separated, it is thus achieved that two substrates with atomically flating surface. Described annealing atmosphere can select according to actual needs, can be oxygen, Ar gas, nitrogen or normal atmospheric atmosphere. Described annealing temperature can select according to substrate, can be 400 DEG C～1200 DEG C. In the present embodiment, described annealing atmosphere is oxygen. Described annealing temperature is 1000 DEG C-1100 DEG C.
In annealing process, although two described burnishing surfaces can make the pollutant in air or surface adsorption thing be mixed between two described burnishing surfaces when directly fitting in dry conditions unavoidably, but it is annealed processing relative to pre-processed substrate is directly exposed to high temperature stove fire by prior art, due to described burnishing surface completely overlapped and contact setting in annealing process of two described pre-processed substrate, greatly reduce the impurity particle pollution to described burnishing surface in annealing atmosphere, additionally, the described burnishing surface of two pre-processed substrate is arranged because of completely overlapped and contact, described burnishing surface fits together almost in contact with less than the gas in annealing furnace, making the outside of the described burnishing surface of a described pre-processed substrate is the body phase of another described pre-processed substrate, and then the gradient difference of the material component in outside no longer exists in each described burnishing surface, body phase material is suppressed to the migration at described burnishing surface place, also may refrain from the material evaporation to gaseous state, it is possible to prevent on described burnishing surface the precipitation of self impurity, and single terminal surface can be formed at described burnishing surface.
When two described pre-processed substrate described burnishing surface in a solvent completely overlapped arrange time, there is between the described burnishing surface of two described pre-processed substrate one layer of solvent membrane, this solvent membrane evaporates along with the rising of temperature in annealing process, the described burnishing surface that can make two described pre-processed substrate fits together closely, such that it is able to avoid the impurity particle pollution to described burnishing surface in annealing atmosphere, it is to avoid pre-processed substrate is directly exposed to the pollution to pre-processed substrate surface that in high temperature stove fire, annealing causes by prior art; Additionally, two described burnishing surfaces of laminating are all not exposed to gas closely, making the outside of the described burnishing surface of a described pre-processed substrate is the body phase of another described pre-processed substrate, and then the gradient difference of the material component in outside no longer exists in each described burnishing surface, body phase material is suppressed to the migration at described burnishing surface place, also may refrain from the material evaporation to gaseous state, it is possible to prevent the precipitation of self impurity on described burnishing surface, and single terminal surface can be formed at described burnishing surface.
Further, stacking arranges the quantity of described pre-processed substrate and is not limited to two, as long as guaranteeing that the described burnishing surface of adjacent described pre-processed substrate is relative and completely overlapped setting, the quantity of described pre-processed substrate can be multiple.
Embodiment 1
Two SrTiO with burnishing surface are provided3Substrate, after being sequentially placed in acetone, isopropanol, ultra-pure water each ultrasonic five minutes to be carried out, by SrTiO3After substrate hot bath is soaked 1 hour, it is placed in the hot hydrochloric acid (HCl) that concentration is 10% and soaks 45 minutes, it is thus achieved that two SrTiO3Pre-processed substrate. By two SrTiO3Pre-processed substrate is stacking in pure water, makes two SrTiO3The burnishing surface of pre-processed substrate relatively and overlaps, it is thus achieved that a laminate structure. Above-mentioned laminate structure is placed in high temperature furnace, after annealing 3 hours at the temperature of 1080 DEG C under oxygen atmosphere, is easily separated, it is thus achieved that two SrTiO with atomically flating surface3Substrate.
Comparative example 1
One SrTiO with burnishing surface is provided3Substrate, after being sequentially placed in acetone, isopropanol, ultra-pure water each ultrasonic five minutes to be carried out, by SrTiO3Substrate is placed in the hot hydrochloric acid that concentration is 10% and soaks 45 minutes, it is thus achieved that a SrTiO after being placed on hot bath immersion 1 hour3Pre-processed substrate. By above-mentioned SrTiO3Pre-processed substrate is placed in high temperature furnace, after annealing 3 hours at the temperature of 1080 DEG C under oxygen atmosphere, it is thus achieved that the SrTiO after a process3Substrate.
Refer to the SrTiO with atomically flating surface that Fig. 2, Fig. 2 (a) obtain for this case embodiment 13Reflection high energy electron spectrum (RHEED) figure, Fig. 2 (b) on (001) surface of substrate is the SrTiO after comparative example 1 process3(001) surface of substrate reflection high energy electron spectrum (RHEED) figure, comparison diagram 2(a) and Fig. 2 (b) it can be seen that this case embodiment 1 acquisition the SrTiO with atomically flating surface3(001) surface of substrate is relative to the SrTiO after comparative example 1 process3(001) striated surface of substrate is clear, sharp-pointed, and the SrTiO with atomically flating surface that this case embodiment 1 obtains is described3The periodicity of (001) surface atom arrangement of substrate 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 obtains3The surface of substrate defines single terminal surface; SrTiO after the process that comparative example 1 obtains3Substrate surface generates ledge structure, and step place forms double; two terminal surface.
Embodiment 2
There is provided two MgO substrates with burnishing surface, after being sequentially placed in acetone, isopropanol, ultra-pure water each ultrasonic five minutes to be carried out, it is thus achieved that two MgO pre-processed substrate. By two MgO pretreatment stackings in pure water, the burnishing surface relative superposition of two MgO pre-processed substrate is made to arrange, it is thus achieved that a laminate structure. Above-mentioned laminate structure is placed in high temperature furnace, after annealing 3 hours at the temperature of 1080 DEG C under oxygen atmosphere, is easily separated, it is thus achieved that two MgO substrates with atomically flating surface.
Comparative example 2
There is provided a MgO substrate with burnishing surface, after being sequentially placed in acetone, isopropanol, ultra-pure water each ultrasonic five minutes to be carried out, it is thus achieved that a MgO pre-processed substrate. This MgO pre-processed substrate is placed in high temperature furnace, anneals 3 hours at 1080 DEG C under oxygen atmosphere, it is thus achieved that the MgO substrate after a process.
Refer to Fig. 5 and Fig. 6, it can be seen that what this case embodiment 2 obtained has the MgO substrate surface cleaning free from admixture on atomically flating surface; MgO substrate surface after comparative example 1 process precipitates out substantial amounts of Ga impurity.
Embodiment 3
Two NdGaO with burnishing surface are provided3Substrate, after being sequentially placed in acetone, isopropanol, ultra-pure water each ultrasonic five minutes to be carried out, by NdGaO3After substrate hot bath is soaked 1 hour, it is placed in the hot hydrochloric acid (HCl) that concentration is 10% and soaks 45 minutes, it is thus achieved that two NdGaO3Pre-processed substrate. By two NdGaO3Pre-processed substrate is stacking in pure water, makes two NdGaO3The burnishing surface of pre-processed substrate relatively and overlaps, it is thus achieved that a laminate structure. Above-mentioned laminate structure is placed in high temperature furnace, after annealing 3 hours at the temperature of 1080 DEG C under oxygen atmosphere, is easily separated, it is thus achieved that two NdGaO with atomically flating surface3Substrate.
Refer to Fig. 7, the NdGaO with atomically flating surface that this case embodiment 3 obtains3The surface of substrate defines single terminal surface.
The preparation method of substrate provided by the invention has the advantages that relative for the burnishing surface of adjacent at least two pre-processed substrate and completely overlapped setting, form a laminate structure, and this laminate structure is placed in high temperature furnace and is annealed process, owing to the burnishing surface of two adjacent pre-processed substrate is because of completely overlapped and contact setting, two adjacent burnishing surfaces fit together almost in contact with less than gas, making the outside of the burnishing surface of a pre-processed substrate is the body phase of pre-processed substrate adjacent thereto, and then the gradient difference of the material component in outside no longer exists in each burnishing surface, body phase material is suppressed to the migration at burnishing surface place, also may refrain from the material evaporation to gaseous state, the precipitation being possible to prevent on burnishing surface self impurity, and single terminal surface can be formed at burnishing surface. further, since the completely overlapped and contact setting in annealing process of the burnishing surface of adjacent two pre-processed substrate, thus decreasing the impurity particle pollution to burnishing surface in atmosphere. the preparation method technique of the substrate with atomically flating surface provided by the invention is simple, be easily achieved and controllability is good.
It addition, those skilled in the art also can do other changes in spirit of the present invention, certainly, these changes done according to present invention spirit, all should be included within present invention scope required for protection.
Claims (10)
1. a preparation method with the substrate on atomically flating surface, the method comprises the following steps:
S10, it is provided that at least two pre-processed substrate of identical material, each described pre-processed substrate has at least one burnishing surface;
S20, arranges formation one laminate structure by described at least two pre-processed substrate stacking, and wherein, the described burnishing surface of two adjacent described pre-processed substrate is relative and completely overlapped setting; And
S30, after being placed in high temperature furnace by described laminate structure to be annealed and processing, separates described laminate structure.
2. the preparation method as claimed in claim 2 with the substrate on atomically flating surface, it is characterised in that the surface roughness of described burnishing surface is 0.5nm ~ 1.5nm.
3. the preparation method as claimed in claim 1 with the substrate on atomically flating surface, it is characterised in that described step S20 comprises the following steps:
S21, soaks described at least two pre-processed substrate in a solvent;
S22, by the relative and completely overlapped setting in described solvent of the described burnishing surface of two adjacent described pre-processed substrate, forms described laminate structure.
4. the preparation method as claimed in claim 3 with the substrate on atomically flating surface, it is characterised in that described solvent is pure water, described pure resistivity of water 18.3M Ω/more than cm.
5. the preparation method as claimed in claim 3 with the substrate on atomically flating surface, it is characterised in that having a pure water film between the described burnishing surface of two adjacent described pre-processed substrate, described pure water film contacts setting with relative two described burnishing surfaces.
6. the preparation method as claimed in claim 1 with the substrate on atomically flating surface, described step S20 comprises the following steps: described at least two pre-processed substrate described burnishing surface whole surface-coated or spray solvent, then by coating or the described at least two pre-processed substrate stacking spraying solvent, make the described burnishing surface of adjacent two and described solvent all be in close contact setting, form described laminate structure.
7. the preparation method as claimed in claim 1 with the substrate on atomically flating surface, it is characterised in that described step S20 comprises the following steps:
S21 ', the described burnishing surface of pre-processed substrate described in cleaning at least two;
S22 ', directly fits in dry conditions by pre-processed substrate described at least two, forms described laminate structure.
8. the preparation method as claimed in claim 1 with the substrate on atomically flating surface, it is characterised in that in described step S21 ', adopts nitrogen gun to purge the described burnishing surface of pre-processed substrate described at least two.
9. the preparation method of the substrate with atomically flating surface stated such as claim 1, it is characterised in that described substrate is strontium titanates substrate, gallic acid neodymium substrate, calcium titanate substrate, lanthanum aluminate substrate or magnesium oxide substrate.
10. the preparation method as claimed in claim 1 with the substrate on atomically flating surface, it is characterised in that described laminate structure is annealed at the temperature of 1000 DEG C-1100 DEG C.
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