CN118169433A - Sub-nano-scale silicon (111) atomic step height standard template and preparation method and application thereof - Google Patents
Sub-nano-scale silicon (111) atomic step height standard template and preparation method and application thereof Download PDFInfo
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 144
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 78
- 239000010703 silicon Substances 0.000 title claims abstract description 75
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 238000005259 measurement Methods 0.000 claims abstract description 31
- 239000000523 sample Substances 0.000 claims abstract description 18
- 238000006073 displacement reaction Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 63
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 28
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 28
- 239000000758 substrate Substances 0.000 claims description 25
- 229920002120 photoresistant polymer Polymers 0.000 claims description 23
- 238000000137 annealing Methods 0.000 claims description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 21
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 21
- 238000005530 etching Methods 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 17
- 238000004140 cleaning Methods 0.000 claims description 10
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 9
- 230000003647 oxidation Effects 0.000 claims description 9
- 238000007254 oxidation reaction Methods 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000010884 ion-beam technique Methods 0.000 claims description 7
- 238000004528 spin coating Methods 0.000 claims description 6
- 238000000151 deposition Methods 0.000 claims description 5
- 238000001312 dry etching Methods 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000007872 degassing Methods 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000011010 flushing procedure Methods 0.000 claims description 4
- 238000007740 vapor deposition Methods 0.000 claims description 4
- 238000010894 electron beam technology Methods 0.000 claims description 3
- 230000005855 radiation Effects 0.000 claims description 3
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 3
- 238000001039 wet etching Methods 0.000 claims description 3
- 238000011161 development Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 238000010586 diagram Methods 0.000 description 5
- 238000009826 distribution Methods 0.000 description 5
- 238000001259 photo etching Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 230000001788 irregular Effects 0.000 description 3
- 238000013508 migration Methods 0.000 description 3
- 230000005012 migration Effects 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
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- 230000008021 deposition Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 230000003252 repetitive effect Effects 0.000 description 1
- 230000010076 replication Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
- C23C16/401—Oxides containing silicon
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/34—Nitrides
- C23C16/345—Silicon nitride
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- 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
- C30B33/005—Oxydation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q40/00—Calibration, e.g. of probes
- G01Q40/02—Calibration standards and methods of fabrication thereof
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Abstract
The invention provides a sub-nano-scale silicon (111) atomic step height standard template, a preparation method and application thereof, wherein the standard template comprises the following steps: the groove is positioned in the middle of the standard template, a plurality of annular atomic steps which are regularly arranged are arranged in the groove, and the height of the annular atomic steps in a single stage is 300-350 pm; the two positioning marks are symmetrically arranged on the outer sides of the annular atomic steps of the outer eaves of the groove, and the positioning marks point to the centers of the annular atomic steps and are used for rapidly determining the positions of the steps to be detected. The standard template can realize the controllability of the total height of the step, so that the standard template has wide coverage range of a high measurement value and stable numerical value, the step height can be directly traced to the silicon lattice constant, the introduced measurement uncertainty is reduced, the standard template can be applied to calibrating Z-axis displacement measurement deviation and Z-direction drift of a scanning probe microscope, and the measurement accuracy of the scanning probe microscope is improved.
Description
Technical Field
The invention relates to the technical field of preparation of sub-nanometer geometric standard substances, in particular to a sub-nanometer scale silicon (111) atomic step height standard template, and a preparation method and application thereof.
Background
In modern integrated circuits, critical component dimensions are expected to shrink to the 1 nm range, and even small changes in roughness, film thickness or geometry on the order of nanometers can have an impact on device performance, which requires the application of the most advanced length metering methods on this scale to achieve accurate measurements, which is critical to ensuring device quality. To address this challenge, basic metrology has changed radically in the definition of basic international system of units (SI), 7 basic units have all been defined by constants, and it has been suggested to use the interplanar spacing (d 220＝192.0155714×10-12 m) of single crystal silicon (SI, 220) in a vacuum environment at 22.5 ℃ as a new rice definition replication to provide technical support for accurate measurement of critical dimensions of integrated circuits. Therefore, development of a calibration standard capable of directly tracing to Si lattice parameters is urgently needed, and standardization of nano-scale and sub-nano-scale measurement is completed while new opportunities for SI unit transformation are adapted.
The scanning probe microscope has atomic-level spatial resolution, and is an instrument capable of detecting the surface morphology and roughness of semiconductors or other high-precision elements in the nanometer and sub-nanometer scale range. With the development of nanotechnology, the application of using a scanning probe microscope to perform sub-nanometer measurement is increasing, and in order to ensure the accuracy of the measurement result and the comparability of the measurement results among different units, the scanning probe microscope needs to be calibrated by using a single-atomic-step height standard template with sub-nanometer height.
At present, the national standard of the lowest step height in China is 5nm, the achieved expanded uncertainty is not more than 1.2nm, and the standardized measurement of the sub-nanometer scale cannot be met. The development of the nano step height standard template is based on a top-down technology, and the top-down method is difficult to be used for the development of the smaller-scale step height standard template due to the limitation of surface roughness. Although the atomic step height standard template with sub-nanometer scale can be developed through high temperature annealing or epitaxial growth and other bottom-up processes, the steps on the surface of the standard template are distributed in a strip shape, the distribution is disordered, the step number and the total height of the steps are uncontrollable, and the height measurement range is not clear. And no definite tracking positioning mark exists, and an operator is required to search a step with a good effect to measure in the measuring and calibrating process, so that the repeatability of standard substance measurement is poor, and the practical calibrating application is difficult to meet.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a sub-nano-scale silicon (111) atomic step height standard template and a preparation method and application thereof, and aims to solve the problems of oversized step size, insufficient fineness, disordered distribution, uncontrollable step number and total height of steps, poor measurement repeatability and the like in the existing standard template. The sub-nano-scale silicon (111) atomic step height standard template has definite positioning marks, steps are distributed in an annular regular mode, the number of the steps and the total height are controllable, and the measurement repeatability is good.
The specific invention comprises the following steps:
in a first aspect, the present invention provides a sub-nanoscale silicon (111) atomic step height standard template comprising: the groove is positioned in the middle of the standard template, 1-30 levels of annular atomic steps are arranged in the groove regularly, and the height of the annular atomic steps in a single level is 300-350 pm;
The two positioning marks are symmetrically arranged on the outer side of the annular atomic step of the outer eave of the groove, and the positioning marks point to the center of the annular atomic step and are used for rapidly determining the position of the step to be detected;
wherein the depth of the groove is 100 nm-2 mu m, and the width is 500 nm-200 mu m.
Optionally, the annular atomic step has 3 stages, and the height of the annular atomic step with a single stage is 300-350 pm.
Optionally, the groove is any one of a circle and a regular polygon.
Optionally, the shape of the positioning mark is any one of rectangle, triangle, arrow, number, letter and Chinese character with directivity.
In a second aspect, the present invention provides a method for preparing the sub-nanoscale silicon (111) atomic step height standard template according to the first aspect, where the preparation method includes:
step 1, preparing a silicon oxide or silicon nitride film with the thickness of 100 nm-2 mu m on the surface of a silicon (111) substrate by adopting any one of thermal oxidation and vapor deposition methods;
Step 2, spin-coating a photoresist layer on the surface of the silicon oxide or silicon nitride film, and selectively exposing and developing to obtain a photoresist removing area with the width of 500 nm-200 mu m and exposing the silicon oxide or silicon nitride film;
step 3, etching the silicon oxide or silicon nitride film in the photoresist removing area through an etching process to obtain a groove with the depth of 100 nm-2 mu m and the width of 500 nm-200 mu m on the surface of the silicon (111) substrate, and then removing the residual photoresist and cleaning to obtain a sub-nano-scale silicon (111) atomic step standard template rough plate; the bottom of the groove is the surface of the silicon (111) substrate;
Step 4, placing the sub-nano-scale silicon (111) atomic step standard template rough plate in a vacuum environment with the vacuum degree of less than or equal to 10 -9 Torr, degassing for 10 hours at 600 ℃, and then flushing for 2-3 seconds at 1200 ℃ to remove oxides and water molecules on the surface of a sample; annealing for 1-5 hours at 900-1000 ℃, and cooling to obtain annular atomic steps with 1-30 levels of regular arrangement and 300-350 pm of single-level height in the groove;
and 5, depositing the outer side of the annular atomic step of the groove outer eave by adopting a focused ion beam, or etching the outer side of the annular atomic step of the groove outer eave by adopting an atomic force microscope anodic oxidation process to form two positioning marks symmetrically arranged on the outer side of the annular atomic step of the groove outer eave, and finally obtaining the sub-nano-scale silicon (111) atomic step height standard template.
Optionally, the annealing includes: heating at high temperature; the high-temperature heating method is any one of a current heating method, a radiation heating method and an electron beam heating method.
Alternatively, when the width of the groove is 20 μm and the depth is 200nm, the annealing temperature is 900 ℃ and the time is 2 hours, the annular atomic step 2 has 3 steps, and the height of the annular atomic step in a single stage is 314pm.
Optionally, the cleaning is an RCA cleaning,
Or ultrasonic cleaning with one or more of isopropyl alcohol, acetone, absolute ethyl alcohol and deionized water.
Optionally, the etching process is any one of a wet etching process and a dry etching process.
In a third aspect, the present invention provides an application of the sub-nanoscale silicon (111) atomic step height standard template according to the first aspect or the sub-nanoscale silicon (111) atomic step height standard template prepared by the preparation method according to the second aspect; the standard template is used for calibrating Z-axis displacement measurement deviation and Z-direction drift of the scanning probe microscope so as to improve measurement accuracy of the scanning probe microscope.
Compared with the prior art, the invention has the following advantages:
(1) According to the sub-nano-scale silicon (111) atomic step height standard template provided by the invention, the silicon (111) substrate is provided with the grooves, the sub-nano-scale annular atomic steps are regularly arranged in the grooves, the number of the steps is controllable, and the controllability of the total height of the steps can be realized. By designing different step levels, a series of step height values can be obtained, so that the coverage range of the height value of the standard template is wide, the value is stable, the step height can be directly traced to the silicon lattice constant, and the introduced measurement uncertainty is reduced. The outer sides of the annular atomic steps of the outer eaves of the grooves are symmetrically provided with positioning marks for rapidly determining the positions of the steps to be detected and ensuring good repeatability of the height values.
(2) According to the preparation method of the sub-nano-scale silicon (111) atomic step height standard template, silicon oxide or silicon nitride films are covered on the surface of a silicon (111) substrate, grooves with the depth of 100 nm-2 mu m and the width of 500 nm-200 mu m are obtained on the surface of the silicon substrate through a photoetching process and an etching process, and finally the standard template is obtained through annealing treatment. According to the invention, the film formed by silicon oxide or silicon nitride material is added on the surface of the silicon (111) material, so that a groove is obtained, and the groove carries out boundary constraint on migration movement of silicon atoms in the high-temperature annealing process at 900-1000 ℃, so that the silicon atom reconstruction arrangement mode on the surface of the silicon (111) substrate is controlled, and the original single-atom step arrangement mode is optimized from irregular strip arrangement to regular annular arrangement; the step number can be controlled by controlling the three-dimensional size of the groove, the high-temperature annealing time and the temperature, so that the controllability of the total height of the step is realized. The invention directly obtains the patterned positioning mark by adopting the focused ion beam or atomic force microscope anodic oxidation process, omits the pattern transfer steps of photoetching, etching and the like, can directly define the pattern, has high positioning precision and improves the processing efficiency. In addition, the atomic step height standard template can calibrate Z-axis displacement measurement deviation and Z-direction drift of the scanning probe microscope, and is beneficial to improving the measurement accuracy of the scanning probe microscope.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 shows a schematic structural diagram of a sub-nanoscale silicon (111) atomic step height standard template provided by an embodiment of the present invention;
FIG. 2 shows a flow chart of a method for preparing a sub-nanoscale silicon (111) atomic step height standard template provided by an embodiment of the invention;
fig. 3 shows a schematic diagram of a process for preparing a sub-nanoscale silicon (111) atomic step height standard template according to an embodiment of the present invention.
Reference numerals illustrate:
1-grooves; 2-ring atomic steps; 3-locating marks.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. The following description of at least one exemplary embodiment is merely exemplary in nature and is in no way intended to limit the invention, its application, or uses. Any product that is the same as or similar to the present invention, which anyone in the light of the present invention or combines the present invention with other prior art features, falls within the scope of the present invention based on the embodiments of the present invention. And all other embodiments that may be made by those of ordinary skill in the art without undue burden and without departing from the scope of the invention.
Specific experimental steps or conditions are not noted in the examples and may be performed in accordance with the operation or conditions of conventional experimental steps described in the prior art in the field. The reagents used, as well as other instruments, are conventional reagent products available commercially, without the manufacturer's knowledge. Furthermore, the drawings are merely schematic illustrations of embodiments of the invention and are not necessarily drawn to scale. The same reference numerals in the drawings denote the same or similar parts, and thus a repetitive description thereof will be omitted. Some of the block diagrams shown in the figures are functional entities and do not necessarily correspond to physically or logically separate entities.
Techniques, methods, and apparatus known to one of ordinary skill in the relevant art may not be discussed in detail, but should be considered part of the specification where appropriate.
In addition, the technical features of the different embodiments of the present invention described below may be combined with each other as long as they do not collide with each other.
In the prior art, when a scanning probe microscope is calibrated by using a step height standard template, the used mature step height standard template is of a micro-nano scale and cannot meet the standardized measurement of a sub-nano scale. Although the atomic step height standard template with sub-nanometer scale can be developed through high temperature annealing or epitaxial growth technology, the standard template has the defects of disordered step distribution, uncontrollable step progression and total step height, poor measurement repeatability and difficulty in meeting the practical calibration application, so that the atomic step height standard template with sub-nanometer scale, which has definite positioning marks, regular step distribution and controllable step quantity and total height, is lacking. Under the background, the silicon oxide or silicon nitride film with specific thickness is covered on the surface of the silicon substrate, the groove with specific size is arranged on the surface of the silicon substrate through the photoetching process and the etching process, the migration movement of silicon atoms is subjected to boundary constraint in the high-temperature annealing process, and the temperature and time of vacuum annealing are controlled, so that the silicon atom reconstruction arrangement mode of the surface of the silicon (111) substrate is controlled, annular atomic steps which are regularly arranged in the groove are obtained, and finally, the positioning mark is arranged at the edge of the annular atomic steps through the focused ion beam or atomic force microscope anodic oxidation process, so that the sub-nanoscale silicon (111) atomic step height standard template with definite positioning mark, step regular distribution, step number and total height controllable is obtained, and the problems in the prior art are solved.
The specific embodiments are as follows:
In a first aspect, the present invention provides a standard template for sub-nanoscale silicon (111) atomic step height, fig. 1 shows a schematic structural diagram of the standard template for sub-nanoscale silicon (111) atomic step height provided in the embodiment of the present invention, where the standard template includes a groove 1, the groove 1 is located in the middle of the standard template, annular atomic steps 2 in 1-30 stages are regularly arranged in the groove 1, and the height of the annular atomic step 2 in a single stage is 300-350 pm;
The two positioning marks 3 are symmetrically arranged on the outer sides of the annular atomic steps 2 of the outer eaves of the groove 1, and the positioning marks 3 point to the centers of the annular atomic steps 2 and are used for rapidly determining the positions of the steps to be detected;
wherein the depth of the groove 1 is 100 nm-2 mu m, and the width is 500 nm-200 mu m.
In some embodiments, the annular atomic step 2 has 3 steps, and the annular atomic step 2 has a height of 314pm.
The groove 1 is any one of a circle and a regular polygon.
The shape of the positioning mark 3 is any one of rectangle, isosceles triangle, arrow, number, letter and Chinese character with directivity.
In a second aspect, the present invention provides a method for preparing a standard template for sub-nanoscale silicon (111) atomic step height according to the first aspect, fig. 2 shows a flowchart of a method for preparing a standard template for sub-nanoscale silicon (111) atomic step height according to an embodiment of the present invention, and as shown in fig. 2, the method includes:
And 1, preparing a silicon oxide or silicon nitride film with the thickness of 100 nm-2 mu m on the surface of a silicon (111) substrate by adopting any one of thermal oxidation and vapor deposition methods.
In the specific implementation of this step, the surface of the silicon (111) material is selected as the substrate.
And step 2, spin-coating a photoresist layer on the surface of the silicon oxide or silicon nitride film, and selectively exposing and developing to obtain a photoresist removing area with the width of 500 nm-200 mu m and exposing the silicon oxide or silicon nitride film.
When the step is implemented, a photoresist layer is uniformly spin-coated on the surface of the silicon oxide or silicon nitride film, and a photoresist removing area with the width of 500 nm-200 mu m and exposing the silicon oxide or silicon nitride film is obtained at the middle position of the silicon substrate through selective exposure and development. The region may be circular or regular polygonal.
Step 3, etching the silicon oxide or silicon nitride film in the photoresist removing area through an etching process to obtain a groove 1 with the depth of 100 nm-2 mu m and the width of 500 nm-200 mu m on the surface of the silicon (111) substrate, and then removing the residual photoresist and cleaning to obtain a sub-nano-scale silicon (111) atomic step standard template rough plate; the bottom of the groove 1 is the surface of the silicon (111) substrate.
When the step is specifically implemented, the etching process is any one of a wet etching process and a dry etching process. The cleaning is RCA cleaning or ultrasonic cleaning with one or more of isopropyl alcohol, acetone, absolute ethyl alcohol and deionized water.
Step4, placing the sub-nano-scale silicon (111) atomic step standard template rough plate in a vacuum environment with the vacuum degree of less than or equal to 10 -9 Torr, degassing for 10 hours at 600 ℃, and then flushing for 2-3 seconds at 1200 ℃ to remove surface oxides and water molecules; and annealing for 1-5 hours at 900-1000 ℃, and cooling to obtain the annular atomic step 2 with 1-30 levels of regular arrangement and 300-350 pm of single-level height in the groove 1.
When this step is carried out, the annealing includes: heating at high temperature; the high-temperature heating method is any one of a current heating method, a radiation heating method and an electron beam heating method.
When the width of the groove is 20 mu m and the depth is 200nm, the annealing temperature is 900 ℃ and the time is 2 hours, the silicon atom reconstruction arrangement mode on the surface of Si (111) is changed, the arrangement mode of single-atom steps is optimized from irregular strip arrangement to regular annular arrangement, the number of steps is controllable, and therefore the controllability of the total height of the steps is realized. The finally obtained annular atomic step 2 has 3 stages, the height of the single-stage annular atomic step is 314pm, the single-stage annular atomic step just corresponds to the lattice parameter value of Si (111), the scale reaches the sub-nanometer level, the high-level value covers 314 pm-942 pm, the value is stable, the source can be directly traced to the lattice constant of the Si, and the introduced measurement uncertainty is reduced.
And 5, depositing the outer side of the annular atomic step 2 of the outer eave of the groove 1 by adopting a focused ion beam, or etching the outer side of the annular atomic step 2 of the outer eave of the groove 1 by adopting an atomic force microscope anodic oxidation process to form two positioning marks 3 symmetrically arranged on the outer side of the annular atomic step 2 of the outer eave of the groove 1, thereby finally obtaining the sub-nano-scale silicon (111) atomic step height standard template.
When the step is specifically implemented, the shape of the positioning mark 3 is any one of rectangle, isosceles triangle, arrow, number, letter and Chinese character with directivity. The position of the tested step can be rapidly determined by combining the groove and the positioning mark, so that the measured value is ensured to have good repeatability.
According to the sub-nano-scale silicon (111) atomic step height standard template, a silicon oxide or silicon nitride film is deposited on the surface of a silicon (111) substrate to form a dielectric layer so as to promote the formation of annular atomic steps 2 which are arranged regularly, and photoresist removal areas which are 500 nm-200 mu m in width and expose the silicon oxide or silicon nitride film are obtained through spin coating photoresist, selective exposure and development. Then removing the silicon oxide or silicon nitride film in the area through etching process, removing photoresist, and obtaining the groove 1 with the depth of 100 nm-2 μm and the width of 500 nm-200 μm at the middle position of the surface of the silicon substrate. Finally, by annealing treatment at specific temperature and time, annular atomic steps 2 with single-stage heights of sub-nanometer level are formed in the grooves 1 in a regular arrangement. The annular atomic step 2 has controllable height and wide coverage range of height values, and the single-stage step height value is the same as the silicon lattice parameter, so that the measurement certainty can be obviously improved.
In a third aspect, the present invention provides an application of the sub-nanoscale silicon (111) atomic step height standard template according to the first aspect or the sub-nanoscale silicon (111) atomic step height standard template prepared by the preparation method according to the second aspect; the standard template is used for calibrating Z-axis displacement measurement deviation and Z-direction drift of the scanning probe microscope so as to improve measurement accuracy of the scanning probe microscope.
In order to make the present invention more clearly understood by those skilled in the art, a sub-nano-scale silicon (111) atomic step height standard template, a method for preparing the same and applications thereof according to the present invention will now be described in detail by the following examples and test examples.
Example 1
A sub-nano-scale silicon (111) atomic step height standard template comprising: the groove 1 is positioned in the middle of the standard template, 1-30 levels of annular atomic steps 2 which are regularly arranged are arranged in the groove 1, 3 levels of annular atomic steps 2 are arranged in the groove 2, and the height of the annular atomic steps 2 in a single level is 314pm;
The two positioning marks 3 are symmetrically arranged on the outer sides of the annular atomic steps 2 of the outer eaves of the groove 1, and the positioning marks 3 point to the centers of the annular atomic steps 2 and are used for rapidly determining the positions of the steps to be detected;
Wherein the depth of the groove 1 is 200nm, and the diameter is 20 mu m;
The groove 1 is circular; the positioning mark 3 is in the shape of an isosceles triangle with directivity;
In this embodiment, the single step height of the standard template for the step height of the Si (111) atom exactly corresponds to the lattice parameter value (314 pm) of the Si (111), and the dimension reaches the sub-nanometer level, so that the uncertainty of the introduced measurement can be reduced. The positioning mark 3 ensures high positioning precision, can rapidly determine the position of the measured step, and ensures high repeatability of the measured value. The annular atomic steps in the atomic step height standard template are regularly arranged, so that Z-axis displacement measurement deviation and Z-direction drift of the scanning probe microscope can be calibrated, and the measurement accuracy of the scanning probe microscope is improved.
Example 2
Based on the same inventive concept, embodiment 2 of the present application provides a method for preparing a sub-nanoscale silicon (111) atomic step height standard template, fig. 3 shows a schematic diagram of a preparation process of the sub-nanoscale silicon (111) atomic step height standard template provided in embodiment 2 of the present application, and as shown in the drawing, a silicon nitride film is deposited on a surface of a silicon substrate, and then spin-coating photoresist, selective exposure and development are performed to obtain a circular photoresist removal region exposing the silicon nitride film. Then removing the silicon nitride film in the area through a dry etching process, removing photoresist, and obtaining a circular groove 1 with specific depth and diameter at the middle position of the surface of the silicon substrate. And then forming annular atomic steps 2 which are regularly arranged in the groove 1 through high-temperature annealing treatment at specific temperature and time. Finally, the positioning mark 3 is obtained by depositing Pt. Specifically, the method comprises the following steps:
Step 1, growing a silicon nitride film with the thickness of 200nm on the surface of a Si (111) substrate by adopting a vapor deposition technology;
Step 2, spin-coating photoresist on the surface of the silicon nitride film, and obtaining a circular photoresist removing area with the diameter of 20 mu m and exposing the silicon nitride film at the middle position of the Si (111) substrate through selective exposure and development;
step 3, etching the silicon nitride film in the circular photoresist removing area through a dry etching process to obtain a groove 1 with the depth of 200nm and the diameter of 20 mu m on the surface of the silicon (111), and then respectively ultrasonically cleaning the groove for 5 minutes by using acetone, absolute ethyl alcohol and deionized water to obtain a sub-nano-scale silicon (111) atomic step standard template rough plate;
And 4, placing the coarse plate of the sub-nano-scale silicon (111) atomic step standard template in a vacuum environment with the vacuum degree of less than 10 - 9 Torr, firstly degassing for 10 hours at 600 ℃, and then flushing for 2-3 seconds at 1200 ℃ to remove oxides, water molecules and other impurities on the surface of the sample. Annealing for 2 hours at 900 ℃, cooling to room temperature, and obtaining annular atomic steps 2 with 3-level regular arrangement and single-level height of 314pm in the groove 1; the high-temperature heating mode in annealing is a current heating method;
And 5, carrying out Pt deposition on the outer side of the uppermost annular atomic step 2 by adopting a focused ion beam process to obtain a positioning mark 3 in the shape of an isosceles triangle, and finally obtaining the sub-nano-scale silicon (111) atomic step height standard template.
According to the preparation method of the sub-nano-scale silicon (111) atomic step height standard template, silicon oxide or silicon nitride materials are added on the surface of a silicon (111) material to form a film, so that grooves are formed, and the grooves carry out boundary constraint on migration movement of silicon atoms in a high-temperature annealing process, so that the silicon atomic reconstruction arrangement mode of the surface of a silicon (111) substrate is controlled, and the original single atomic step arrangement mode is optimized from irregular strip arrangement to regular annular arrangement; the step number can be controlled by controlling the three-dimensional size of the groove, the high-temperature annealing time and the temperature, so that the controllability of the total height of the step is realized. The patterned positioning mark is directly obtained by adopting a focused ion beam or atomic force microscope anodic oxidation process, so that the pattern transferring steps such as photoetching and etching are omitted, patterns can be directly defined, the positioning accuracy is high, and the processing efficiency is improved.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, one skilled in the art can combine and combine the different embodiments or examples described in this specification.
For the purposes of simplicity of explanation, the methodologies are shown as a series of acts, but one of ordinary skill in the art will recognize that the present invention is not limited by the order of acts described, as some acts may, in accordance with the present invention, occur in other orders and concurrently. Further, those skilled in the art will recognize that the embodiments described in the specification are all of the preferred embodiments, and that the acts and components referred to are not necessarily required by the present invention.
The invention provides a sub-nano-scale silicon (111) atomic step height standard template, a preparation method and application thereof, and a specific example is applied to explain the principle and implementation of the invention, and the description of the above example is only used for helping to understand the method and core idea of the invention; meanwhile, as those skilled in the art will have variations in the specific embodiments and application scope in accordance with the ideas of the present invention, the present description should not be construed as limiting the present invention in view of the above.
Claims (10)
1. A sub-nanoscale silicon (111) atomic step height standard template, comprising: the groove is positioned in the middle of the standard template, 1-30 levels of annular atomic steps are arranged in the groove regularly, and the height of the annular atomic steps in a single level is 300-350 pm;
the two positioning marks are symmetrically arranged on the outer sides of the annular atomic steps of the outer eaves of the groove, and the positioning marks point to the centers of the annular atomic steps and are used for rapidly determining the positions of the steps to be detected;
wherein the depth of the groove is 100 nm-2 mu m, and the width is 500 nm-200 mu m.
2. A master template according to claim 1 wherein the annular atomic steps have 3 steps, the height of a single step of the annular atomic steps being 314pm.
3. The master template of claim 1 wherein the grooves are any one of circular and regular polygons.
4. The standard template of claim 1, wherein the positioning mark has a shape of any one of a rectangle, an isosceles triangle, an arrow, a number, a letter, and a kanji having directivity.
5. A method for preparing a sub-nanoscale silicon (111) atomic step height standard template according to any one of claims 1 to 4, comprising:
step 1, preparing a silicon oxide or silicon nitride film with the thickness of 100 nm-2 mu m on the surface of a silicon (111) substrate by adopting any one of thermal oxidation and vapor deposition methods;
Step 2, spin-coating a photoresist layer on the surface of the silicon oxide or silicon nitride film, and selectively exposing and developing to obtain a photoresist removing area with the width of 500 nm-200 mu m and exposing the silicon oxide or silicon nitride film;
step 3, etching the silicon oxide or silicon nitride film in the photoresist removing area through an etching process to obtain a groove with the depth of 100 nm-2 mu m and the width of 500 nm-200 mu m on the surface of the silicon (111) substrate, and then removing the residual photoresist and cleaning to obtain a sub-nano-scale silicon (111) atomic step standard template rough plate; the bottom of the groove is the surface of the silicon (111) substrate;
Step 4, placing the sub-nano-scale silicon (111) atomic step standard template rough plate in a vacuum environment with the vacuum degree of less than or equal to 10 - 9 Torr, degassing for 10 hours at 600 ℃, and then flushing for 2-3 seconds at 1200 ℃ to remove surface oxides and water molecules; annealing for 1-5 hours at 900-1000 ℃, and cooling to obtain annular atomic steps with 1-30 levels of regular arrangement and 300-350 pm of single-level height in the groove;
and 5, depositing the outer side of the annular atomic step of the groove outer eave by adopting a focused ion beam, or etching the outer side of the annular atomic step of the groove outer eave by adopting an atomic force microscope anodic oxidation process to form two positioning marks symmetrically arranged on the outer side of the annular atomic step of the groove outer eave, and finally obtaining the sub-nano-scale silicon (111) atomic step height standard template.
6. The method of making a master template of claim 5 wherein said annealing comprises: heating at high temperature; the high-temperature heating method is any one of a current heating method, a radiation heating method and an electron beam heating method.
7. A method of producing a master template according to claim 5 wherein the ring-shaped atomic step 2 has 3 steps and the ring-shaped atomic step has a single step height of 314pm when the groove has a width of 20 μm and a depth of 200nm, the annealing temperature is 900 ℃ and the time is 2 hours.
8. The method of manufacturing a master template according to claim 5, wherein the cleaning is RCA cleaning,
Or ultrasonic cleaning with one or more of isopropyl alcohol, acetone, absolute ethyl alcohol and deionized water.
9. The method of manufacturing a master template according to claim 5, wherein the etching process is any one of a wet etching process and a dry etching process.
10. Use of a sub-nanoscale silicon (111) atomic step height standard template according to any one of claims 1 to 4 or a sub-nanoscale silicon (111) atomic step height standard template produced by the production method according to any one of claims 5 to 9; the standard template is used for calibrating Z-axis displacement measurement deviation and Z-direction drift of the scanning probe microscope so as to improve measurement accuracy of the scanning probe microscope.
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