CN113532348A - Single line width sample plate structure with magnitude of 22nm and below and preparation method thereof - Google Patents

Single line width sample plate structure with magnitude of 22nm and below and preparation method thereof Download PDF

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CN113532348A
CN113532348A CN202110791794.8A CN202110791794A CN113532348A CN 113532348 A CN113532348 A CN 113532348A CN 202110791794 A CN202110791794 A CN 202110791794A CN 113532348 A CN113532348 A CN 113532348A
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film
layer
sample
film layer
line width
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张易军
闫天怡
王琛英
任巍
蒋庒德
叶作光
王瑞康
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Xian Jiaotong University
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Xian Jiaotong University
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B21/00—Measuring arrangements or details thereof, where the measuring technique is not covered by the other groups of this subclass, unspecified or not relevant
    • G01B21/02—Measuring arrangements or details thereof, where the measuring technique is not covered by the other groups of this subclass, unspecified or not relevant for measuring length, width, or thickness
    • G01B21/04—Measuring arrangements or details thereof, where the measuring technique is not covered by the other groups of this subclass, unspecified or not relevant for measuring length, width, or thickness by measuring coordinates of points
    • G01B21/042—Calibration or calibration artifacts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • 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
    • 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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • 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
    • C23C16/403—Oxides of aluminium, magnesium or beryllium
    • 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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • 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
    • C23C16/405—Oxides of refractory metals or yttrium
    • 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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • 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
    • C23C16/407—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
    • 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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • 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
    • C23C16/44—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 method of coating
    • C23C16/455—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 method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45523—Pulsed gas flow or change of composition over time
    • C23C16/45525—Atomic layer deposition [ALD]
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B21/00—Measuring arrangements or details thereof, where the measuring technique is not covered by the other groups of this subclass, unspecified or not relevant
    • G01B21/02—Measuring arrangements or details thereof, where the measuring technique is not covered by the other groups of this subclass, unspecified or not relevant for measuring length, width, or thickness

Abstract

A single line width sample plate structure with 22nm and below and its preparation method, including substrate layer, first film layer, second film layer and tie coat; the first film layer and the second film layer are sequentially arranged on the substrate layer from top to bottom to form film layer units, and the first film layers of the two film layer units are oppositely arranged and are bonded through bonding layers; and grooves with the width less than or equal to 22 nanometers are arranged on the second film layer. The invention utilizes the advantages of the atomic layer deposition technology that the film thickness is accurately controllable in the sub-nanometer level, the process repeatability is high and the like, adopts the design idea of converting the film thickness into the characteristic dimension of the nanometer line width sample plate to prepare the high-precision microscale (the measuring range below 22 nm) nanometer single line width sample plate, and the limit dimension of the high-precision line width prepared at present reaches 16nm, which reaches the top level in China and the top level in the world.

Description

Single line width sample plate structure with magnitude of 22nm and below and preparation method thereof
Technical Field
The invention belongs to the field of research on standard substances for calibrating a nanometer line width instrument, and particularly relates to a single line width sample plate structure with a magnitude of 22 nanometers or less and a preparation method thereof.
Background
To date, researchers have developed numerous methods for making nano-wire-width templates; line width templates processed by these techniques are mostly in the range of tens of nanometers to a few micrometers. For example: ultraviolet lithography, X-ray lithography, or synchrotron radiation can be used to fabricate nanoscale gratings or line-width templates, but these methods also have their own drawbacks. For ultraviolet lithography, the requirement for exposure light source is often high in order to obtain the limit resolution, and at present, the requirement is 193nm excimer laser, but the technology is difficult to manufacture a nano line width template with the line width less than 100 nm. X-ray lithography is another possible method of preparing a template of the nano-line width, but it requires the use of simultaneous radiation of electrons as a light source, which is expensive and inconvenient.
In addition, these methods require the production of special masks and complex optical lens systems, which means extremely high processing costs. The ultimate resolution of these methods is further enhanced by the use of shorter wavelength light sources, and the lens systems tend to have higher absorption at shorter wavelengths, which is a technical bottleneck.
The Electron Beam Lithography (EBL) method can obtain a high resolution (<10nm), is a direct-write processing method, does not require a mask plate, but has a low manufacturing efficiency and an unavoidable proximity field effect, resulting in a deviation between a design dimension and a finally processed dimension. In recent years, the photoetching technology based on a scanning probe microscope can also be used for preparing the nano-line width template, but the processing speed of the technology is low, and the repeatability is poor.
Disclosure of Invention
The invention aims to provide a single line width sample plate structure with the size of 22 nanometers and below and a preparation method thereof, so as to overcome the defects of high cost, low efficiency or poor repeatability in the preparation process of the existing nanometer line width sample plate.
In order to achieve the purpose, the invention adopts the following technical scheme:
a single linewidth template structure with a magnitude of 22 nanometers and below comprises a substrate layer, a first film layer, a second film layer and a bonding layer; the first film layer and the second film layer are sequentially arranged on the substrate layer from top to bottom to form film layer units, and the first film layers of the two film layer units are oppositely arranged and are bonded through bonding layers; and grooves with the width less than or equal to 22 nanometers are arranged on the second film layer.
Further, the thickness of the first film layer is 400-5000 nm; the thickness of the second film layer is 16-22 nm; the film layer unit is a cube structure with the side length of 2-10 mm; the adhesive layer is epoxy resin.
Further, the first film layer is Al2O3Thin film or HfO2The second film layer is a ZnO film, a ZrO2 film or a TiO2 film, and the substrate layer is single crystal Si, quartz or sapphire;
furthermore, a third film layer or a film layer is etched off on the two film layer units arranged on one surface of the groove so as to regulate and control the characteristic quantity value of the single-line-width sample plate.
Further, a method for preparing a single line width template structure with 22nm and the following values comprises the following steps:
step 1, depositing a micro-scale nanometer double-layer film respectively composed of two different materials on the upper surface of a clean substrate;
step 2, cutting and cleaning the nano double-layer film obtained in the step 1 to form a plurality of cubic blocks;
step 3, butting and pasting every two membrane surfaces of the cubic blocks obtained in the step 2 to form a pair of sticky samples; heating and curing the obtained sticky sample to obtain a cured sample;
step 4, cutting the solidified sample obtained in the step 3 to form a plurality of samples, and grinding the obtained plurality of samples to obtain ground samples;
step 5, performing ion polishing treatment on the grinding sample obtained in the step 4 to obtain a polished sample;
step 6, corroding the polished sample obtained in the step 5 to form a single-line-width sample plate with the adjustable value of 22 nanometers or less;
and 7, according to the actual deviation of the processing value and the set metering value, depositing a three-dimensional uniform nano film with a certain thickness on the upper surface of the nano single-line-width sample plate by utilizing an atomic layer deposition technology or an atomic layer etching technology or etching a layer of film to regulate and control the characteristic quantity value of the single-line-width sample plate.
Further, in step 1, an atomic layer deposition method is adopted for deposition, and the adopted organometallic precursor source is diethyl zinc, dimethyl zinc, tetra (dimethylamino) titanium, tetra (methylamino) hafnium, tetra (dimethylamino) hafnium, tetra (methylamino) zirconium or tetra (dimethylamino) zirconium; the oxygen source used was deionized water (H)2O) and hydrogen peroxide (H)2O2) Oxygen (O)2) Or ozone (O)3) (ii) a The nitrogen source used may be ammonia gas, ammonia plasma, nitrogen gas or nitrogen plasma.
Further, in the step 3, a clamp is used for pressurizing and fixing, and then the product is placed into an oven or a heating table at the temperature of 120-160 ℃ for heating for 0.5-2 hours for curing treatment; in the step 4, during grinding, firstly, the coarse grinding is carried out by using 600-800-mesh water-washing sand paper, and then the fine grinding is carried out by using grinding films of 30 micrometers, 6 micrometers, 1 micrometer and 0.1 micrometer in sequence.
Further, the ion beam polishing in step 5 is to put the sample into a low-angle argon ion beam and bombard the sample to be polished for 30-90 minutes by using an incident angle of 5-12 degrees and energy of 1-8 keV.
Further, in the step 6, the etching solution used in the etching process is an acidic solution with a volume ratio of 1:100-1:10000, and the etching time is 5-5000 seconds.
Further, the specific process of step 7 is as follows: and (3) correcting the growth/etching rate according to the previous growth/etching result, performing atomic layer deposition/etching on the upper surface of the single-line-width sample plate in the step (6), firstly closing an exhaust valve connected between a vacuum pump and the reaction cavity, performing 1 st precursor source pulse, opening the exhaust valve for 5-100 seconds by using 50-200sccm nitrogen to purge the exhaust valve after 1-100 seconds of 1 st precursor pulse completion, then performing 2 nd source pulse, opening the exhaust valve for 5-100 seconds by using 50-200sccm nitrogen to purge the exhaust valve after 1-100 seconds of 2 nd precursor pulse completion, and sequentially circulating until the preset thickness value of growth/etching is completed.
Compared with the prior art, the invention has the following technical effects:
according to the single linewidth sample plate with the magnitude of 22 nanometers and below and the preparation method thereof, the ALD technology with the best film thickness control and three-dimensional uniformity is utilized to prepare the nano double-layer film with the accurate thickness, and then the micro-nano processing technologies such as cutting, gluing, grinding and polishing and the like are utilized to convert the thickness of the nano film into the characteristic size of the nano linewidth sample plate, so that the technical limit that the traditional photoetching and etching technology cannot process the nano linewidth sample plate with the minimum size is broken through, the processing accuracy and repeatability of the nano linewidth sample plate can be greatly improved, and the method has important significance for preparing the high-accuracy and high-quality nano linewidth sample plate. The method is simple and easy in preparation process, is compatible with the existing industrialized semiconductor preparation process flow, can prepare a high-quality micro-scale nano line width sample plate with low cost and simple equipment, and finally realizes the preparation of the micro-scale value adjustable nano single line width sample plate with the size of 16nm-22 nm.
Furthermore, when the characteristic dimension of the obtained single-line-width sample plate with the adjustable value of 22 nanometers and below does not meet the process requirement, the characteristic dimension of the single-line-width sample plate is corrected by depositing a film with a certain thickness on the upper surface of the single-line-width sample plate by using an atomic layer deposition method or etching the atomic layer, so that the technical bottleneck that the processing error and the characteristic value cannot be corrected after the traditional nanometer line-width sample plate is formed at one time is broken. Because the atomic layer deposition technology has good three-dimensional uniformity, a uniform and conformal film can be deposited on the three-dimensional micro-scale nano line width sample plate, and further the characteristic values of the sample plates are regulated or corrected. Because the atomic layer deposition technology has good three-dimensional uniformity, uniform and conformal films can be deposited on the image grid and the three-dimensional micro-scale nano line width sample plate, and further the characteristic values of the sample plates are regulated or corrected.
The invention utilizes the advantages of the atomic layer deposition technology that the film thickness is accurately controllable in the sub-nanometer level, the process repeatability is high and the like, adopts the design idea of converting the film thickness into the characteristic dimension of the nanometer line width sample plate to prepare the high-precision microscale (the measuring range below 22 nm) nanometer single line width sample plate, and the limit dimension of the high-precision line width prepared at present reaches 16nm, which reaches the top level in China and the top level in the world.
Drawings
FIG. 1 is a flow chart of a 22nm and below adjustable single line width template and fabrication for atomic force and scanning electron microscope calibration;
FIG. 2 is an SEM image of a 16nm line width template prepared by the method of the present invention;
FIG. 3 is an SEM image of a 22nm line width template prepared by the method of the present invention;
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
The invention provides a single line width sample plate with 22nm and the following values and a preparation method thereof, comprising the following steps:
step 1, depositing a micro-scale nano double-layer film which is respectively formed by two different materials and has accurately controllable thickness on the upper surface of a clean substrate by utilizing an atomic layer deposition method;
wherein, the organometallic precursor source used in the atomic layer deposition method is diethyl zinc, dimethyl zinc, tetra (dimethylamino) titanium, tetra (methylamino) hafnium, tetra (dimethylamino) hafnium, tetra (methylamino) zirconium or tetra (dimethylamino) zirconium.
The oxygen source used was deionized water (H)2O) and hydrogen peroxide (H)2O2) Oxygen (O)2) Or ozone(O3)。
The nitrogen source used can be ammonia gas, ammonia plasma, nitrogen gas, nitrogen plasma and the like.
Step 2, cutting the nano double-layer film obtained in the step 1 into squares with the side length of 2-10mm, and cleaning the surface;
step 3, the film ends of the two small squares are butted and stuck by using epoxy resin for the small squares obtained in the step 2, the stuck samples are pressurized and fixed by using a special clamp, and then the samples are placed into an oven or a heating table at the temperature of 120-160 ℃ for heating for 0.5-2 hours for curing treatment;
step 4, cutting the sample bonded and cured in the step 3 into a small cuboid sample divided into two parts by a wire saw, adhering the sample to the upper surface of a balance grinding table by using a hot melt adhesive side for grinding to obtain a ground sample, wherein in the grinding process, firstly, 600-plus 800-mesh water-washing abrasive paper is used for carrying out coarse grinding, and then, grinding films of 30 micrometers, 6 micrometers, 1 micrometer and 0.1 micrometer are sequentially used for carrying out fine grinding;
step 5, performing ion beam polishing treatment on the grinding sample obtained in the step 4 to obtain a polished sample, wherein the polishing process condition is that the sample is placed in a low-angle argon ion beam, and bombarding the sample to be polished for 30-90 minutes by using the energy of 1-8keV and the incident angle of 5-12 degrees; (ii) a
Step 6, etching the polished sample obtained in the step 5 for 5-5000 seconds, selectively etching off one of the nano double-layer films to form a sample plate with adjustable single line width of 22 nanometers and below;
and 7, if the characteristic dimension of the single-line width sample plate with the adjustable 22nm and the following values obtained in the step 6 does not meet the process requirement, correcting the sample plate by using an atomic layer deposition/etching method, wherein the specific process comprises the following steps: and (3) correcting the growth/etching rate according to the previous growth/etching result, performing atomic layer deposition/etching on the upper surface of the single-line-width sample plate in the step (6), firstly closing an exhaust valve connected between a vacuum pump and the reaction cavity, performing 1 st precursor source pulse, opening the exhaust valve for 5-100 seconds by using 50-200sccm nitrogen to purge the exhaust valve after 1-100 seconds of 1 st precursor pulse completion, then performing 2 nd source pulse, opening the exhaust valve for 5-100 seconds by using 50-200sccm nitrogen to purge the exhaust valve after 1-100 seconds of 2 nd precursor pulse completion, and sequentially circulating until the preset thickness value of growth/etching is completed.
Example 1
The invention provides a single line width sample plate with 22nm and the following values and a preparation method thereof, comprising the following steps:
1) cleaning a single crystal Si substrate by using an RCA standard cleaning process and purging the surface of the single crystal Si substrate by using dry nitrogen for later use;
2) sending the single crystal Si substrate processed in the step 1 into an atomic layer deposition system through a vacuum loading mechanical arm of the atomic layer deposition system, and heating to 200-300 ℃ to prepare for depositing a thin film material;
3) based on step 2, diethyl zinc and deionized water (H) are used2O) respectively serving as Zn precursor sources and O precursor sources, and depositing a ZnO film with the thickness of 16nm on the surface of the single crystal Si by utilizing an ALD (atomic layer deposition) technology; the deposition process parameters are as follows: the pulse time of the zinc is 0.1-0.3 seconds, and the nitrogen cleaning is carried out for 5.0-10.0 seconds after the pulse is finished; the second pulse is deionized water, the pulse time of the deionized water is 0.1-0.2 seconds, and the pulse is completed and then nitrogen cleaning is carried out for 6.0-12.0 seconds;
4) adopting trimethylaluminum and deionized water (H) on the basis of the step 32O) are respectively used as Al and O precursor sources, and Al with the thickness of 400-5000nm is deposited on the surface of a silicon wafer with 16nm zinc oxide grown by utilizing the ALD technology2O3A film; the deposition process parameters are as follows: the first pulse is trimethylaluminum, the pulse time is 0.1-0.3 seconds, and the nitrogen cleaning is carried out after the pulse is finished and immediately follows 5.0-10.0 seconds; the second pulse is deionized water, the pulse time of the deionized water is 0.1-0.2 seconds, and the pulse is completed and then nitrogen cleaning is carried out for 6.0-12.0 seconds;
5) cutting the nano double-layer film obtained in the step 4 into squares of 4mmx4mm, cleaning the surface, mixing imported epoxy resin G1 glue and a curing agent according to the mass ratio of 4:1, and butting and adhering the end faces of the two small squares of the film;
6) pressurizing and fixing the adhered sample in the step 5, and heating the sample in an oven or a heating table at 120-160 ℃ for 1 hour for curing;
7) cutting the sample adhered and cured in the step 6 into a small cuboid sample with the size of 2mm x4mm by using a fretsaw, and then adhering the sample to the upper surface of a balance grinding table by using a hot melt adhesive side for grinding to obtain a ground sample; grinding: firstly, coarse grinding is carried out by using 600-800-mesh water-washing abrasive paper, and then fine grinding is carried out by using grinding thin films of 30 micrometers, 6 micrometers, 1 micrometer and 0.1 micrometer in sequence;
8) performing ion beam polishing treatment on the grinding sample obtained in the step 7 to obtain a polished sample; specifically, the method comprises the following steps: putting the sample in the step 7 into a low-angle argon ion beam, and bombarding the sample to be polished for 30-90 minutes by using an incident angle of 5-12 degrees and energy of 1-8 keV;
9) and (3) putting the polished sample obtained in the step (8) into a weak acid solution prepared by 36-38% of hydrochloric acid and deionized water according to the volume ratio of 1:100-1:10000, corroding for 5-5000 seconds, generating height difference in the nano double-layer film, and forming a 16-nanometer-magnitude adjustable nano single-groove line width sample plate.
10) And when the characteristic dimension of the 16-nanometer-magnitude adjustable nanometer single-groove line width sample plate obtained in the step 9 does not meet the requirement, correcting the growth speed according to the growth result, and growing a uniform and conformal thin film on the upper surface of the nanometer single-groove line width sample plate structure by using ALD (atomic layer deposition) or regulating the characteristic dimension of the microscale line width sample plate by using atomic layer etching.
As shown in fig. 2, which is an SEM image of a line width sample plate with a thickness of 16nm, it can be seen from the figure that the line width characteristic value of the prepared line width sample plate is 16nm, which is very uniform.
Example 2
The invention provides a single line width sample plate with 22nm and the following values and a preparation method thereof, comprising the following steps:
1) cleaning a single crystal Si substrate by using an RCA standard cleaning process and purging the surface of the single crystal Si substrate by using dry nitrogen for later use;
2) sending the single crystal Si substrate processed in the step 1 into an atomic layer deposition system through a vacuum loading mechanical arm of the atomic layer deposition system, and heating to 200-300 ℃ to prepare for depositing a thin film material;
3) based on step 2, diethyl zinc and deionized water (H) are used2O) respectively serving as Zn precursor sources and O precursor sources, and depositing a ZnO film with the thickness of 22nm on the surface of the single crystal Si by utilizing an ALD (atomic layer deposition) technology; the deposition process parameters are as follows: the pulse time of the zinc is 0.1-0.3 seconds, and the nitrogen cleaning is carried out for 5.0-10.0 seconds after the pulse is finished; the second pulse is deionized water, the pulse time of the deionized water is 0.1-0.2 seconds, and the pulse is completed and then nitrogen cleaning is carried out for 6.0-12.0 seconds;
4) adopting trimethylaluminum and deionized water (H) on the basis of the step 32O) are respectively used as Al and O precursor sources, and Al with the thickness of 400-5000nm is deposited on the surface of a silicon wafer with 22nm zinc oxide grown by utilizing the ALD technology2O3A film; the deposition process parameters are as follows: the first pulse is trimethylaluminum, the pulse time is 0.1-0.3 seconds, and the nitrogen cleaning is carried out after the pulse is finished and immediately follows 5.0-10.0 seconds; the second pulse is deionized water, the pulse time of the deionized water is 0.1-0.2 seconds, and the pulse is completed and then nitrogen cleaning is carried out for 6.0-12.0 seconds;
5) cutting the nano double-layer film obtained in the step 4 into squares of 4mmx4mm, cleaning the surface, mixing imported epoxy resin G1 glue and a curing agent according to the mass ratio of 4:1, and butting and adhering the end faces of the two small squares of the film;
6) pressurizing and fixing the adhered sample in the step 5, and heating the sample in an oven or a heating table at 120-160 ℃ for 1 hour for curing;
7) cutting the sample adhered and cured in the step 6 into a small cuboid sample with the size of 2mm x4mm by using a fretsaw, and then adhering the sample to the upper surface of a balance grinding table by using a hot melt adhesive side for grinding to obtain a ground sample; grinding: firstly, coarse grinding is carried out by using 600-800-mesh water-washing abrasive paper, and then fine grinding is carried out by using grinding thin films of 30 micrometers, 6 micrometers, 1 micrometer and 0.1 micrometer in sequence;
8) performing ion beam polishing treatment on the grinding sample obtained in the step 7 to obtain a polished sample; specifically, the method comprises the following steps: putting the sample in the seventh step into a low-angle argon ion beam, and bombarding the sample to be polished for 30-90 minutes by using the energy of 1-8keV and the incident angle of 5-12 degrees;
9) and (3) putting the polished sample obtained in the step (8) into a weak acid solution prepared by 36-38% of hydrochloric acid and deionized water according to the volume ratio of 1:100-1:10000, corroding for 5-5000 seconds, generating height difference in the nano double-layer film, and forming a 22-nanometer-magnitude adjustable nano single-groove line width sample plate.
10) And when the characteristic dimension of the 22-nanometer-magnitude adjustable nanometer single-groove line width sample plate obtained in the step 9 does not meet the requirement, correcting the growth speed according to the growth result, and growing a uniform and conformal thin film on the upper surface of the nanometer single-groove line width sample plate structure by using ALD (atomic layer deposition) or regulating the characteristic dimension of the microscale line width sample plate by using atomic layer etching.
As shown in fig. 3, which is an SEM image of a line width sample with a thickness of 22nm in a micro-scale nano line width sample, it can be seen that the line width characteristic value of the prepared line width sample is 22nm, which is very uniform.
In conclusion, the method of the present invention prepares a micro-scale nano double-layered thin film having a precise thickness using the ALD technique that is best in terms of film thickness control and three-dimensional uniformity, and then, by cutting, for micro-nano processing technologies such as adhesion, grinding and polishing, the thickness of the nano film is converted into the characteristic dimension of the nano line width sample plate, not only breaks through the technical limit that the traditional photoetching and etching technology can not process the small-size nanometer line width sample plate, but also greatly improves the processing accuracy and the repeatability of the nanometer line width sample plate, and also breaks through the technical bottleneck that the processing error and the characteristic value of the traditional nanometer line width sample plate after one-step forming can not be corrected, which has important significance for preparing the high-accuracy and high-quality nanometer line width sample plate, through the work, the preparation of the micro-scale nanometer line width sample plate with the thickness of 16-22nm is realized, and the level which is top in China and the leading level in the world is reached. The method has simple and easy preparation process, is compatible with the existing industrialized semiconductor preparation process flow, can prepare high-quality micro-scale nanometer line width sample plates by using low-cost and simple equipment, has wide industrial application in the fields of integrated circuits, national defense and military industry, advanced manufacturing, biological medicine and the like, and fundamentally leads the nanometer metering standard device in China to reach the world advanced level.

Claims (10)

1. A single linewidth template structure with a magnitude of 22 nanometers and below is characterized by comprising a substrate layer, a first film layer, a second film layer and a bonding layer; the first film layer and the second film layer are sequentially arranged on the substrate layer from top to bottom to form film layer units, and the first film layers of the two film layer units are oppositely arranged and are bonded through bonding layers; and grooves with the width less than or equal to 22 nanometers are arranged on the second film layer.
2. The template structure of claim 1, wherein the thickness of the first film layer is 400-5000 nm; the thickness of the second film layer is 16-22 nm; the film layer unit is a cube structure with the side length of 2-10 mm; the adhesive layer is epoxy resin.
3. The template structure of claim 1, wherein the first layer is Al2O3Thin film or HfO2The second film layer is a ZnO film, a ZrO2 film or a TiO2 film, and the substrate layer is single crystal Si, quartz or sapphire.
4. The template structure of claim 1, wherein the feature value of the single-line-width template is adjusted by providing a third layer on the two film units on the side where the grooves are formed or etching away a thin film.
5. A method for preparing a single line width template structure with a size of 22nm and below, based on any one of claims 1 to 4, comprising the steps of:
step 1, depositing a micro-scale nanometer double-layer film respectively composed of two different materials on the upper surface of a clean substrate;
step 2, cutting and cleaning the nano double-layer film obtained in the step 1 to form a plurality of cubic blocks;
step 3, butting and pasting every two membrane surfaces of the cubic blocks obtained in the step 2 to form a pair of sticky samples; heating and curing the obtained sticky sample to obtain a cured sample;
step 4, cutting the solidified sample obtained in the step 3 to form a plurality of samples, and grinding the obtained plurality of samples to obtain ground samples;
step 5, performing ion polishing treatment on the grinding sample obtained in the step 4 to obtain a polished sample;
step 6, corroding the polished sample obtained in the step 5 to form a single-line-width sample plate with the adjustable value of 22 nanometers or less;
and 7, according to the actual deviation of the processing value and the set metering value, depositing a three-dimensional uniform nano film with a certain thickness on the upper surface of the nano single-line-width sample plate by utilizing an atomic layer deposition technology or an atomic layer etching technology or etching a layer of film to regulate and control the characteristic quantity value of the single-line-width sample plate.
6. The method of claim 5, wherein step 1, depositing is performed by atomic layer deposition, and the organometallic precursor source is diethylzinc, dimethylzinc, tetrakis (dimethylamino) titanium, tetrakis (methylamino) hafnium, tetrakis (dimethylamino) hafnium, tetrakis (methylamino) zirconium, or tetrakis (dimethylamino) zirconium; the oxygen source used was deionized water (H)2O) and hydrogen peroxide (H)2O2) Oxygen (O)2) Or ozone (O)3) (ii) a The nitrogen source used may be ammonia gas, ammonia plasma, nitrogen gas or nitrogen plasma.
7. The method for preparing a single line width template structure with a size of 22nm and below according to claim 5, wherein the step 3 is performed by pressing and fixing with a clamp, and then the template structure is placed in an oven or a heating table with a temperature of 120 ℃ to 160 ℃ to be heated for 0.5 to 2 hours for curing treatment; in the step 4, during grinding, firstly, the coarse grinding is carried out by using 600-800-mesh water-washing sand paper, and then the fine grinding is carried out by using grinding films of 30 micrometers, 6 micrometers, 1 micrometer and 0.1 micrometer in sequence.
8. The method as claimed in claim 5, wherein the step 5 of ion beam polishing comprises exposing the sample to a low angle argon ion beam, and bombarding the sample to be polished at an incident angle of 5 ° -12 ° and an energy of 1-8keV for 30-90 min.
9. The method as claimed in claim 5, wherein in step 6, the etching solution is an acidic solution with a volume ratio of 1:100-1:10000, and the etching time is 5-5000 seconds.
10. The method as claimed in claim 5, wherein the step 7 comprises the following steps: and (3) correcting the growth/etching rate according to the previous growth/etching result, performing atomic layer deposition/etching on the upper surface of the single-line-width sample plate in the step (6), firstly closing an exhaust valve connected between a vacuum pump and the reaction cavity, performing 1 st precursor source pulse, opening the exhaust valve for 5-100 seconds by using 50-200sccm nitrogen to purge the exhaust valve after 1-100 seconds of 1 st precursor pulse completion, then performing 2 nd source pulse, opening the exhaust valve for 5-100 seconds by using 50-200sccm nitrogen to purge the exhaust valve after 1-100 seconds of 2 nd precursor pulse completion, and sequentially circulating until the preset thickness value of growth/etching is completed.
CN202110791794.8A 2021-07-13 2021-07-13 Single line width sample plate structure with magnitude of 22nm and below and preparation method thereof Pending CN113532348A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1786655A (en) * 2005-12-20 2006-06-14 西安交通大学 Nano Line width sample plate and its preparation method
CN110306168A (en) * 2019-07-02 2019-10-08 西安交通大学 A kind of controllable periodic nanometer line width template of characteristic size and preparation method thereof
CN110530313A (en) * 2019-07-26 2019-12-03 西安交通大学 One kind is across multiple dimensioned line width standard of magnitude and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1786655A (en) * 2005-12-20 2006-06-14 西安交通大学 Nano Line width sample plate and its preparation method
CN110306168A (en) * 2019-07-02 2019-10-08 西安交通大学 A kind of controllable periodic nanometer line width template of characteristic size and preparation method thereof
CN110530313A (en) * 2019-07-26 2019-12-03 西安交通大学 One kind is across multiple dimensioned line width standard of magnitude and preparation method thereof

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Application publication date: 20211022