CN106917067A - A kind of method of regulation and control magnetic Nano ring size - Google Patents
A kind of method of regulation and control magnetic Nano ring size Download PDFInfo
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- CN106917067A CN106917067A CN201710190508.6A CN201710190508A CN106917067A CN 106917067 A CN106917067 A CN 106917067A CN 201710190508 A CN201710190508 A CN 201710190508A CN 106917067 A CN106917067 A CN 106917067A
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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
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- 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
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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
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5826—Treatment with charged particles
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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
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5873—Removal of material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/14—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates
- H01F41/18—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates by cathode sputtering
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/14—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates
- H01F41/30—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates for applying nanostructures, e.g. by molecular beam epitaxy [MBE]
Abstract
The invention discloses a kind of method of regulation and control magnetic Nano ring size.Magnetic Nano ring in the present invention is prepared using polystyrene microsphere template method, monodispersed polystyrene microsphere is prepared on substrate first, then one layer of nonmagnetic film and thin magnetic film are deposited respectively on substrate using the method for magnetron sputtering deposition film, recycle ion etching technology carries out ion milling to the film for preparing, so as to form monodispersed magnetic Nano ring structure sample.In the process, by adjusting the size of polystyrene microsphere and the thickness of non magnetic transition zone, it is possible to achieve the regulation and control to object construction magnetic Nano ring size, including magnetic Nano ring external diameter, internal diameter and ring width regulation and control;The regulation and control to magnetic Nano ring thickness can be realized by the control to the magnetosphere thin film sputtering time.The method process is simple, it is convenient and reliable, the magnetic Nano ring of various sizes and material can be prepared, meet different experiment needs and scientific researches.
Description
Technical field
The present invention relates to technical field of nano material, especially a kind of method of regulation and control magnetic Nano ring size.
Background technology
The magnetic material of nano-scale plays more and more important effect in many devices.This material is each due to its
From unique shape and size determine in it magnetized state and Magnetic moment reversal characteristic, important work is played in many devices
With.Nano-rings as a kind of very special nano material, due on its high symmetry and structure geometrically from
Closure, shows many properties, such as resistance with outer field oscillation Aharonov-Bhom effects, to magnetic field or electric field
Sensitive nano-antenna, the shell level structure with similar electron outside nucleus, the surface plasma of near infrared region frequency-adjustable
Excimer.If introducing magnetic, nano-rings can show more rich physics, chemical property, for example its can be formed two kinds it is very steady
Fixed magnetic state:Vortex state and double farmlands state, the Quantum Transport property in ferromagnetic nanometer ring;Huge magnetoelectricity in ferromagnetic nanometer ring
Inhibition effect and spin-transfer torque effect, and as perpendicular magnetic random-access memory unit etc..These characteristics make its light, electricity, magnetic,
The fields such as catalysis, information Store and microwave absorption are with a wide range of applications.The performance of nano-rings mainly by ring pattern,
The influence of size, composition and quality.Magnetized state particularly in nano-rings, such as vortex state and double farmlands state, between them
Change depending on nano-rings internal-and external diameter size and thickness and material property in itself.
The content of the invention
For above-mentioned problem, it is an object of the invention to provide a kind of method of regulation and control magnetic Nano ring size.
The technical scheme is that:A kind of method of regulation and control magnetic Nano ring size, comprises the following steps:
Step one:Choose a kind of substrate of substrate as film sample, cut growth 10mm, width 10mm, thickness 0.5mm it is big
It is small;Acetone ultrasonic wave cleans 10-15min, then cleans 10-15min with deionized water ultrasonic wave, finally uses absolute ethyl alcohol ultrasonic wave
Cleaning 10-15min, takes out the drying of substrate high pure nitrogen standby after cleaning up;
Step 2:A kind of polystyrene microsphere emulsion is chosen, according to emulsion and deionized water volume ratio 1:200 are diluted
Afterwards, the ultrasonic disperse 10-15min in ultrasonic cleaner, makes polystyrene microsphere fully dispersed;By scattered polystyrene
Microspheres solution is dropped on the substrate cleaned up in step one, is dried in placement drying box;
Step 3:After substrate is fully dried, put it into magnetron sputtering chamber, it is first on substrate with magnetically controlled sputter method
Non magnetic transition zone is deposited, be positioned over substrate in ion etching instrument by redeposited one layer of thin magnetic film, and ion is carried out to film
It is thinning;Because Properties of Polystyrene Nano Particles is organic material, it is difficult to etch, and polystyrene microsphere has scattering to imitate in etching ion
Should, so polystyrene microsphere will be played to the thin-film material below it blocking or protective effect, it is to avoid film by high energy from
Son is etched away completely.And the part do not blocked by polystyrene microsphere, film will be etched completely away, so in polystyrene
The magnetic Nano structure of ring-type, i.e. magnetic Nano ring can be formed around Nano microsphere.Polystyrene microsphere as needed whether, use
Acetone soln washes it from substrate, obtains magnetic Nano ring.
Further, the substrate in the step 2 is placed in drying box with the horizontal 15 ° of angles and dries, drying box temperature
Degree maintains 55 DEG C.
Further, the material of the magnetic Nano ring is any one in iron, cobalt, nickel simple substance ferromagnetic metal, or
It is any one in the ferromagnetic alloy material with iron, cobalt, nickel as matrix, or any one in ferromagnetic oxide.
Further, the non magnetic buffer layer material is nonmagnetic metal, non-magnetic insulator, or other non magnetic conjunctions
Gold, oxide material.
Further, the substrate material is non-magnetic insulator material.
Compared with prior art, the beneficial effects of the invention are as follows:The magnetic Nano ring regulates and controls method process is simple, according to need
Ask, by controlling the size of polystyrene microsphere and the thickness of nonmagnetic layer, the magnetic that can prepare various sizes and material is received
Meter Huan, meets different experiment needs and scientific researches.
Brief description of the drawings
Fig. 1 is the preparation method schematic diagram of controllable sized magnetic nano-rings of the invention.
Fig. 2 is that the present invention prepares magnetic Nano using the polystyrene microsphere and the non magnetic transition zones of 20nm of diameter 200nm
The schematic diagram of ring.
Fig. 3 is that the present invention prepares magnetic Nano using the polystyrene microsphere and the non magnetic transition zones of 20nm of diameter 500nm
The schematic diagram of ring.
Fig. 4 is that the present invention prepares magnetic Nano using the polystyrene microsphere and the non magnetic transition zones of 60nm of diameter 500nm
The schematic diagram of ring.
The polystyrene microsphere of the monodispersed diameter 200nm prepared on Fig. 5 substrates.
The cobalt ferromagnetic nanometer ring that Fig. 6 is prepared using the non magnetic transition zone of polystyrene microsphere and 20nm of diameter 200nm.
Fig. 7 is received using permalloy magnetic prepared by the non magnetic transition zone of polystyrene microsphere and 20nm of diameter 500nm
Meter Huan.
Fig. 8 is received using permalloy magnetic prepared by the non magnetic transition zone of polystyrene microsphere and 60nm of diameter 500nm
Meter Huan.
Specific embodiment
In the description of the invention, it is to be understood that term " " center ", " longitudinal direction ", " transverse direction ", " on ", D score,
The orientation or position relationship of the instruction such as "front", "rear", "left", "right", " vertical ", " level ", " top ", " bottom ", " interior ", " outward " are
Based on orientation shown in the drawings or position relationship, it is for only for ease of and describes the present invention and simplify to describe, rather than instruction or dark
Showing the device or element of meaning must have specific orientation, with specific azimuth configuration and operation therefore it is not intended that right
Limitation of the invention.Additionally, term " first ", " second " etc. are only used for describing purpose, and it is not intended that indicating or implying phase
To importance or the implicit quantity for indicating indicated technical characteristic.Thus, the feature for defining " first ", " second " etc. can
To express or implicitly include one or more this feature.In the description of the invention, unless otherwise indicated, " multiple "
It is meant that two or more.
The present invention is further illustrated with reference to the accompanying drawings and examples.
Embodiment 1
The present embodiment is to regulate and control ferro-cobalt magnetic with the polystyrene microsphere of 200 nanometers of diameter and 20 nanometers of non magnetic transition zones
The size of nano-rings, as depicted in figs. 1 and 2, comprises the following steps:
(1) the thick silica thin slices of 0.5mm are chosen, the thin slice of 10mm × 10mm is cut into as insulating substrate,
Substrate is cleaned as medium using acetone, deionized water and absolute ethyl alcohol using ultrasonic wave successively, by substrate high pure nitrogen
Drying is standby;
(2) the Properties of Polystyrene Nano Particles emulsion of diameter 200nm is chosen, polystyrene microsphere emulsion presses body with deionized water
Product compares 1:200 are diluted, and being then placed in ultrasonic cleaner carries out fully dispersed, and the operating power of ultrasonic cleaner is
100W.After through dilution and ultrasonic disperse, scattered polystyrene microsphere solution is dropped in the titanium dioxide handled well in step (1)
On silicon chip, then it is positioned in drying box, substrate keeps 15 ° of angles in drying box with horizontal plane, drying box temperature maintains 55
℃。
(3) substrate is put into magnetron sputtering plating, coating chamber is extracted into 2 × 10-5The vacuum of Pascal, is splashed with magnetic control
Shooting method is first in deposition on substrate 20nm thick copper metal film as non magnetic transition zone, redeposited one layer of 40nm thick ferro-cobalt
Magnetosphere, working gas is the argon gas of 0.5Pa.Then take out, substrate is positioned in ion etching instrument, etching instrument vacuum is taken out
To 5 × 10-4Pa, then passes to argon gas, keeps operating air pressure 2 × 10-2Pa.It is ion energy to set ion etch process parameter
450eV, beam current density is 0.5mA/cm2, vertical thinning, thinning process is carried out to film after keeping 5min to make ion beam current stabilization
Middle sample stage rotational velocity 9rpm, the working time is 2min.
Substrate is taken out after the completion of etching, is put into acetone soln and is cleaned by ultrasonic 2min, the polystyrene on removal substrate is micro-
Ball, that is, obtain ferro-cobalt magnetic Nano ring.
The size of the cobalt ferromagnetic nanometer ring for preparing is as follows:
The external diameter of magnetic Nano ring:D=200nm, internal diameter:
Width:W=(D-d)/2=20nm, thickness t=40nm.
The ferro-cobalt that Fig. 6 is prepared for the non magnetic transition zone of polystyrene microsphere and 20nm in embodiment 1 using 200nm
The stereoscan photograph of magnetic Nano ring, nanometer ring size is external diameter 195nm, internal diameter 162nm, width 16.5nm.
Embodiment 2
The non magnetic transition zone regulation and control permalloy magnetic of polystyrene microsphere and 20nm of the present embodiment diameter 500nm is received
The size of meter Huan, as shown in figures 1 and 3, comprises the following steps:
(1) the thick quartz glass of 0.5mm is chosen, the thin slice of 10mm × 10mm is cut into as insulating substrate, by base
Piece is cleaned as medium using acetone, deionized water and absolute ethyl alcohol using ultrasonic wave successively, is dried up with high pure nitrogen by substrate
It is standby;
(2) the Properties of Polystyrene Nano Particles emulsion of diameter 500nm is chosen, polystyrene microsphere emulsion presses body with deionized water
Product compares 1:200 are diluted, and being then placed in ultrasonic cleaner carries out fully dispersed, and the operating power of ultrasonic cleaner is
100W.After through dilution and ultrasonic disperse, scattered polystyrene microsphere solution is dropped in the quartzy glass handled well in step (1)
On glass substrate, then it is positioned in drying box, substrate keeps 15 ° of angles in drying box with horizontal plane, drying box temperature maintains 55
℃。
(3) substrate is put into magnetron sputtering plating, coating chamber is extracted into 2 × 10-5The vacuum of Pa, uses magnetron sputtering side
First in deposition on substrate 20nm thick silica membrane as non magnetic transition zone, redeposited one layer of 40nm thick perm is closed method
Golden magnetosphere (such as Fig. 3), working gas is the argon gas of 0.5Pa, is then taken out, and substrate is positioned in ion etching instrument, is etched
Instrument vacuum is evacuated to 5 × 10-4Pa, then passes to argon gas, keeps operating air pressure 2 × 10-2Pa.Ion etch process parameter is set
It is ion energy 450eV, beam current density is 0.5mA/cm2, film is vertically subtracted after keeping 5min to make ion beam current stabilization
It is thin, sample stage rotational velocity 9rpm in thinning process, the working time is 2min.
Substrate is taken out after the completion of etching, is put into acetone soln and is cleaned by ultrasonic 2min, the polystyrene on removal substrate is micro-
Ball, that is, obtain permalloy magnetic Nano ring.
The size of the permalloy magnetic Nano ring for preparing is as follows:
The external diameter of magnetic Nano ring:D=500nm, internal diameter:
Width:W=(D-d)/2=115nm, thickness t=40nm.
The permalloy that Fig. 7 is prepared for the non magnetic transition zone of polystyrene microsphere and 20nm in embodiment 2 using 500nm
The stereoscan photograph of magnetic Nano ring, nanometer ring size is external diameter 520nm, internal diameter 272nm, width 124nm.
Embodiment 3
The non magnetic transition zone regulation and control permalloy magnetic of polystyrene microsphere and 60nm of the present embodiment diameter 500nm is received
The size of meter Huan, as shown in Figure 1 and Figure 4, comprises the following steps:
(1) the thick quartz glass of 0.5mm is chosen, the thin slice of 10mm × 10mm is cut into as insulating substrate, by base
Piece is cleaned as medium using acetone, deionized water and absolute ethyl alcohol using ultrasonic wave successively, is dried up with high pure nitrogen by substrate
It is standby;
(2) the Properties of Polystyrene Nano Particles emulsion of diameter 500nm is chosen, polystyrene microsphere emulsion presses body with deionized water
Product compares 1:200 are diluted, and being then placed in ultrasonic cleaner carries out fully dispersed, and the operating power of ultrasonic cleaner is
100W.After through dilution and ultrasonic disperse, scattered polystyrene microsphere solution is dropped in the quartzy glass handled well in step (1)
On glass substrate, then it is positioned in drying box, substrate keeps 15 ° of angles in drying box with horizontal plane, drying box temperature maintains 55
℃。
(3) substrate is put into magnetron sputtering plating, coating chamber is extracted into 2 × 10-5The vacuum of Pa, uses magnetron sputtering side
First in deposition on substrate 60nm thick silica membrane as non magnetic transition zone, redeposited one layer of 40nm thick perm is closed method
Golden magnetosphere (such as Fig. 4), working gas is the argon gas of 0.5Pa, is then taken out, and substrate is positioned in ion etching instrument, is etched
Instrument vacuum is evacuated to 5 × 10-4Pa, then passes to argon gas, keeps operating air pressure 2 × 10-2Pa.Ion etch process parameter is set
It is ion energy 450eV, beam current density is 0.5mA/cm2, film is vertically subtracted after keeping 5min to make ion beam current stabilization
It is thin, sample stage rotational velocity 9rpm in thinning process, the working time is 2min.
Substrate is taken out after the completion of etching, is put into acetone soln and is cleaned by ultrasonic 2min, the polystyrene on removal substrate is received
Meter Wei Qiu, that is, obtain permalloy magnetic Nano ring.
The size of the permalloy magnetic Nano ring for preparing is as follows:
The external diameter of magnetic Nano ring:D=500nm, internal diameter:
Width:W=(D-d)/2=66.5nm, thickness t=40nm.
The permalloy that Fig. 8 is prepared for the non magnetic transition zone of polystyrene microsphere and 60nm in embodiment 3 using 500nm
The stereoscan photograph of magnetic Nano ring, nanometer ring size is external diameter 518nm, internal diameter 370nm, width 74nm.
With above-mentioned according to desirable embodiment of the invention as enlightenment, by above-mentioned description, relevant staff is complete
Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention
Property scope is not limited to the content on specification, it is necessary to its technical scope is determined according to right.
Claims (5)
1. it is a kind of regulate and control magnetic Nano ring size method, it is characterised in that comprise the following steps:
Step one:Choose a kind of substrate of substrate as film sample, cut growth 10mm, width 10mm, the size of thickness 0.5mm;
Acetone ultrasonic wave cleans 10-15min, then cleans 10-15min with deionized water ultrasonic wave, finally clear with absolute ethyl alcohol ultrasonic wave
10-15min is washed, the drying of substrate high pure nitrogen is taken out after cleaning up standby;
Step 2:A kind of polystyrene microsphere emulsion is chosen, according to emulsion and deionized water volume ratio 1:After 200 are diluted,
The ultrasonic disperse 10-15min in ultrasonic cleaner, makes polystyrene microsphere fully dispersed;Scattered polystyrene is micro-
Ball solution is dropped on the substrate cleaned up in step one, is dried in placement drying box;
Step 3:After substrate is fully dried, put it into magnetron sputtering chamber, with magnetically controlled sputter method first in deposition on substrate
Non magnetic transition zone, redeposited one layer of thin magnetic film, substrate is positioned in ion etching instrument, and carrying out ion to film subtracts
It is thin;The magnetic Nano structure of ring-type, i.e. magnetic Nano ring are formed around Properties of Polystyrene Nano Particles.Polystyrene microsphere according to
Whether need, it is washed from substrate with acetone soln, obtain magnetic Nano ring.
2. it is according to claim 1 it is a kind of regulate and control magnetic Nano ring size method, it is characterised in that in the step 2
Substrate be placed in drying box with the horizontal 15 ° of angles and dry, drying box temperature maintains 55 DEG C.
3. it is according to claim 1 it is a kind of regulate and control magnetic Nano ring size method, it is characterised in that the magnetic Nano
The material of ring is any one in iron, cobalt, nickel simple substance ferromagnetic metal, or the ferromagnetic alloy with iron, cobalt, nickel as matrix
Any one in material, or any one in ferromagnetic oxide.
4. it is according to claim 1 it is a kind of regulate and control magnetic Nano ring size method, it is characterised in that the non magnetic mistake
It is nonmagnetic metal, non-magnetic insulator, other nonmagnetic alloys or oxide material to cross layer material.
5. it is according to claim 1 it is a kind of regulate and control magnetic Nano ring size method, it is characterised in that the substrate material
It is non-magnetic insulator material.
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CN113913766A (en) * | 2021-10-20 | 2022-01-11 | 杭州电子科技大学 | Preparation method of nano-structure array with controllable morphology |
CN114231928A (en) * | 2021-12-22 | 2022-03-25 | 杭州电子科技大学 | Preparation method of annular stepped nanostructure |
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CN113913766A (en) * | 2021-10-20 | 2022-01-11 | 杭州电子科技大学 | Preparation method of nano-structure array with controllable morphology |
CN114231928A (en) * | 2021-12-22 | 2022-03-25 | 杭州电子科技大学 | Preparation method of annular stepped nanostructure |
CN114231928B (en) * | 2021-12-22 | 2023-12-29 | 杭州电子科技大学 | Preparation method of annular stepped nano structure |
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