CN113120857A - Preparation method of optical micro-nano structure - Google Patents

Preparation method of optical micro-nano structure Download PDF

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Publication number
CN113120857A
CN113120857A CN202110400994.6A CN202110400994A CN113120857A CN 113120857 A CN113120857 A CN 113120857A CN 202110400994 A CN202110400994 A CN 202110400994A CN 113120857 A CN113120857 A CN 113120857A
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layer
ion beam
nano structure
optical micro
silicon
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欧欣
王成立
伊艾伦
沈晨
张加祥
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Shanghai Institute of Microsystem and Information Technology of CAS
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Shanghai Institute of Microsystem and Information Technology of CAS
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B81MICROSTRUCTURAL TECHNOLOGY
    • B81CPROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C1/00Manufacture or treatment of devices or systems in or on a substrate
    • B81C1/00015Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
    • B81C1/00023Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems without movable or flexible elements
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B81MICROSTRUCTURAL TECHNOLOGY
    • B81CPROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C1/00Manufacture or treatment of devices or systems in or on a substrate
    • B81C1/00436Shaping materials, i.e. techniques for structuring the substrate or the layers on the substrate
    • B81C1/00523Etching material
    • B81C1/00531Dry etching
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/002Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of materials engineered to provide properties not available in nature, e.g. metamaterials
    • G02B1/005Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of materials engineered to provide properties not available in nature, e.g. metamaterials made of photonic crystals or photonic band gap materials

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  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Nanotechnology (AREA)
  • Analytical Chemistry (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Optics & Photonics (AREA)
  • Optical Integrated Circuits (AREA)

Abstract

The application relates to a preparation method of an optical micro-nano structure, which comprises the steps of obtaining a heterogeneous composite substrate; the heterogeneous composite substrate sequentially comprises a thin film layer, an insulating layer and a supporting substrate from top to bottom; the thin film layer is made of silicon material; carrying out ion beam cutting on the heterogeneous composite substrate to obtain an optical micro-nano structure; the optical micro-nano structure comprises a damaged layer caused by ion beam cutting, and the damaged layer is positioned on the thin film layer; annealing the optical micro-nano structure to form a silicon dioxide layer at the position of the damaged layer; the thickness of the silicon dioxide layer is larger than that of the damage layer; and removing the silicon dioxide layer to remove the damaged layer together to obtain the undamaged optical micro-nano structure. Therefore, the damage of the ion beam to the material can be effectively removed, and the high-performance optical micro-nano structure is obtained.

Description

Preparation method of optical micro-nano structure
Technical Field
The application relates to the technical field of semiconductor preparation, in particular to a preparation method of an optical micro-nano structure.
Background
The preparation method of the micro-nano structure comprises ion beam processing, extreme ultraviolet interference photoetching, hole mask colloid photoetching, thermal evaporation and the like, wherein the most utilized method is the ion beam processing. The ion beam processing Micro-nano structure has the characteristics of simplicity, convenience and rapidness, and is widely applied to the fields of transmission electron microscope sample preparation, optical structure processing, surface polishing, Micro Electro Mechanical Systems (MEMS) and the like.
The application of ion beams to the preparation of optical structures often faces the problem of material damage. During ion beam processing, a large number of high energy focused ions bombard the material lattice to remove material, and at the same time, the ions are implanted into the material to form a damaged layer, which causes optical absorption, resulting in large optical propagation loss of the processed optical device.
The damage layer generally comprises lattice distortion and amorphous material, and traditionally, can make the damage layer obtain the restoration to a certain extent through annealing, and the principle is: firstly, under the condition of high temperature, atoms of a substance move, so that regularly arranged crystal lattices are spontaneously reformed; ② ions implanted by the ion beam will diffuse under high temperature and escape to the outside. However, this annealing method does not completely remove the damage caused by ion beam bombardment.
Therefore, how to completely remove the damage layer caused by ion beam bombardment is a key problem of ion beam processing optical devices.
Disclosure of Invention
The embodiment of the application provides a preparation method of an optical micro-nano structure, an oxide layer is formed in a damaged layer at a high temperature, then the oxide layer is removed, damage caused by ion beams can be effectively removed, and the process flow is simple and convenient.
The embodiment of the application provides a preparation method of an optical micro-nano structure, which comprises the following steps:
obtaining a heterogeneous composite substrate; the heterogeneous composite substrate sequentially comprises a thin film layer, an insulating layer and a supporting substrate from top to bottom; the thin film layer is made of silicon material;
carrying out ion beam cutting on the heterogeneous composite substrate to obtain an optical micro-nano structure; the optical micro-nano structure comprises a damaged layer caused by ion beam cutting, and the damaged layer is positioned on the thin film layer;
annealing the optical micro-nano structure to form a silicon dioxide layer at the position of the damaged layer; the thickness of the silicon dioxide layer is larger than that of the damage layer;
and removing the silicon dioxide layer to remove the damaged layer together to obtain the undamaged optical micro-nano structure.
Optionally, after obtaining the heterogeneous composite substrate, before performing ion beam cutting on the heterogeneous composite substrate, the method further includes:
and forming a protective layer on the surface of the thin film layer.
Optionally, after the ion beam cutting is performed on the heterogeneous composite substrate, before the annealing treatment is performed on the optical micro-nano structure, the method further includes:
and placing the heterogeneous composite substrate and the protective layer after the ion beam cutting into an etching solution to remove the protective layer.
Optionally, the protective layer is made of a metal material;
the metal material includes at least one of chromium, nickel, titanium, and gold.
Optionally, the protective layer is made of a non-metallic material;
the non-metallic material includes at least one of silicon oxide, silicon nitride, titanium oxide, and aluminum oxide.
Optionally, the silicon material is silicon or silicon carbide.
Optionally, the ion beam is any one of a gallium ion beam, a silicon ion beam, a helium ion beam, and a boron ion beam;
the energy of the ion beam is 1-100 keV; the beam current of the ion beam is 0.1 pA-100 nA.
Optionally, the annealing temperature range is 200-1300 ℃;
the annealing atmosphere is at least one of argon, nitrogen, oxygen and atmospheric atmosphere.
Optionally, the etching solution includes hydrofluoric acid or a buffered oxide etching solution.
Optionally, the optical micro-nano structure is any one of a micro-ring, a micro-disk, an optical waveguide and a photonic crystal.
The preparation method of the optical micro-nano structure provided by the embodiment of the application has the following beneficial effects:
obtaining a heterogeneous composite substrate; the heterogeneous composite substrate sequentially comprises a thin film layer, an insulating layer and a supporting substrate from top to bottom; the thin film layer is made of silicon material; carrying out ion beam cutting on the heterogeneous composite substrate to obtain an optical micro-nano structure; the optical micro-nano structure comprises a damaged layer caused by ion beam cutting, and the damaged layer is positioned on the thin film layer; annealing the optical micro-nano structure to form a silicon dioxide layer at the position of the damaged layer; the thickness of the silicon dioxide layer is larger than that of the damage layer; and removing the silicon dioxide layer to remove the damaged layer together to obtain the undamaged optical micro-nano structure. Therefore, the damage of the ion beam to the material can be effectively removed, and the high-performance optical micro-nano structure is obtained.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
Fig. 1 is a schematic flow chart of a method for manufacturing an optical micro-nano structure provided in an embodiment of the present application;
fig. 2 is a schematic diagram of a preparation process of an optical micro-nano structure provided in an embodiment of the present application;
fig. 3 is a schematic diagram of a preparation process of another optical micro-nano structure provided in an embodiment of the present application;
fig. 4 is a comparative diagram of an optical transmission curve provided in an embodiment of the present application.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
It should be noted that the terms "first," "second," and the like in the description and claims of this application and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the application described herein are capable of operation in sequences other than those illustrated or described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or server that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
In order to improve the quality factor of a photonic structure etched by an ion beam, a damaged layer caused by ion beam bombardment needs to be completely removed.
A specific embodiment of a method for manufacturing an optical micro-nano structure according to the present application is described below, fig. 1 is a schematic flow chart of a method for manufacturing an optical micro-nano structure according to the embodiment of the present application, and the present specification provides method operation steps according to the embodiment or the flow chart, but more or fewer operation steps may be included based on conventional or non-inventive labor. The order of steps recited in the embodiments is merely one manner of performing the steps in a multitude of orders and does not represent the only order of execution. In conjunction with the schematic preparation process shown in fig. 2, the method may include:
s101: as shown in fig. 2(a), a hetero-composite substrate 1 is obtained; the heterogeneous composite substrate 1 sequentially comprises a thin film layer 11, an insulating layer 12 and a supporting substrate 13 from top to bottom; the thin film layer 11 is made of a silicon material;
s103: as shown in fig. 2(b), performing ion beam cutting on the heterogeneous composite substrate 1 to obtain an optical micro-nano structure; the optical micro-nano structure comprises a damaged layer 14 caused by ion beam cutting, and the damaged layer 14 is positioned on the thin film layer 11;
s105: as shown in fig. 2(c), annealing the optical micro-nano structure to form a silicon dioxide layer 15 at the position of the damaged layer 14; the thickness of the silicon dioxide layer 15 is greater than the thickness of the damaged layer 14;
s107: as shown in fig. 2(d), the silicon dioxide layer 15 is removed to remove the damaged layer 14 together, and an undamaged optical micro-nano structure is obtained.
In the embodiment of the application, considering that in the ion beam cutting process, part of ions penetrate into the surface and the side wall of the thin film layer 11 to form the damaged layer 14, that is, the defects of the ion beam are located at the edge of the structure, in the annealing process, silicon in the damaged layer 14 is oxidized into silicon dioxide, so that the silicon dioxide layer 15 is formed at the edge of the structure, and the damaged layer 14 can be removed by removing the silicon dioxide layer 15 through an etching solution; thus, through the steps of S101 to S107, damage of the ion beam to the material can be effectively removed, thereby obtaining a high-performance optical micro-nano structure.
In an alternative embodiment, the silicon material is silicon or silicon carbide.
In an alternative embodiment, the ion beam is any one of a gallium ion beam, a silicon ion beam, a helium ion beam, and a boron ion beam; the energy of the ion beam is 1-100 keV; the beam current of the ion beam is 0.1 pA-100 nA.
In an optional embodiment, the annealing temperature range is 200-1300 ℃; the annealing atmosphere is at least one of argon, nitrogen, oxygen and atmospheric atmosphere.
In an alternative embodiment, the etching solution comprises hydrofluoric acid or Buffered Oxide Etch (BOE) solution.
In an optional embodiment, the optical micro-nano structure is any one of a micro-ring, a micro-disk, an optical waveguide and a photonic crystal.
A specific embodiment of another optical micro-nano structure preparation method according to the present application is described below, and fig. 3 is a schematic diagram of another optical micro-nano structure preparation process according to the present application, where the optical micro-nano structure preparation method according to the present application may include:
s101: as shown in fig. 3(a), a hetero-composite substrate 1 is obtained; the heterogeneous composite substrate 1 sequentially comprises a thin film layer 11, an insulating layer 12 and a supporting substrate 13 from top to bottom; the thin film layer 11 is made of a silicon material;
s102: as shown in fig. 3(b), a protective layer 2 is formed on the surface of the thin film layer 11.
S103: as shown in fig. 3(c), performing ion beam cutting on the heterogeneous composite substrate 1 and the protective layer 2 to obtain an optical micro-nano structure; the optical micro-nano structure comprises a damaged layer 14 caused by ion beam cutting, and the damaged layer 14 is positioned on the thin film layer 11;
s104: as shown in fig. 3(d), the ion beam cut hetero-composite substrate 1 and the protective layer 2 are placed in an etching solution to remove the protective layer 2.
S105: as shown in fig. 3(e), annealing the optical micro-nano structure to form a silicon dioxide layer 15 at the position of the damaged layer 14; the thickness of the silicon dioxide layer 15 is greater than the thickness of the damaged layer 14;
s107: as shown in fig. 3(f), the damaged layer 14 is removed together by removing the silica layer 15, and an undamaged optical micro-nano structure is obtained.
The preparation method of this embodiment is substantially the same as that of the first embodiment, except that before the ion beam etching, a protective layer 2 is formed in advance through step S102 to protect the top surface of the thin film layer 11 and prevent the ion penetration from causing large-area damage; simultaneously, before annealing, the protective layer 2 is removed by corrosive solution; the embodiment can also achieve the beneficial effects of effectively removing the damage of the ion beam to the material and obtaining the high-performance optical micro-nano structure.
In an alternative embodiment, the protective layer is made of a metallic material; the metal material includes at least one of chromium, nickel, titanium, and gold.
In another alternative embodiment, the protective layer is made of a non-metallic material; the non-metallic material includes at least one of silicon oxide, silicon nitride, titanium oxide, and aluminum oxide.
To further illustrate the utility of the fabrication methods provided herein, the above examples and alternative embodiments of the present invention are further described below with reference to the fabrication of a photonic circular microdisk resonator. Referring to fig. 3, the heterogeneous composite substrate 1 is a silicon carbide film on an insulator, and the method for preparing the whispering gallery microdisk resonator by etching the silicon carbide film on the insulator through ion beams mainly comprises the following steps:
obtaining a silicon carbide film on an insulator, wherein the silicon carbide film comprises a silicon carbide layer 11, a silicon oxide layer 12 and a silicon substrate layer 13;
metal chromium is evaporated on the upper surface of the silicon carbide layer 11 to form a protective layer 2, according to the SRIM simulation, the thickness of the chromium is more than 20nm, so that ions stay in the protective layer 2, and direct bombardment of the subsequent ions on the surface of the silicon carbide layer 11 is avoided; meanwhile, the protective layer 2 can also avoid excessive charge accumulation during ion beam imaging;
fixing the silicon carbide film on the insulator plated with the metal chromium in a sample groove, cutting the chromium layer 2, the silicon carbide layer 11 and the silicon oxide layer 12 by using a focused gallium ion beam, wherein the path of the ion beam is designed to be circular so as to form a circular micro-nano structure; wherein the focused gallium ion beam has an energy of 30keV and a dose of 110pA, and the processing of the ion beam forms a damaged layer 14 in the silicon carbide layer 11, the damaged layer 14 comprising amorphous silicon carbide and severely damaged single crystal silicon carbide;
placing the prepared round micro-nano structure in aqua regia solution until chromium metal is completely removed;
placing the prepared round micro-nano structure in an annealing furnace, annealing for 10 hours at the annealing temperature of 900 ℃, wherein the annealing atmosphere is oxygen atmosphere; the silicon carbide will form a silicon dioxide layer 15 at high temperature, covering the surface and sidewalls of the silicon carbide 11.
And (3) placing the annealed micro-nano structure in a BOE solution, and completely removing the silicon dioxide layer 15 covering the surface and the side wall of the silicon carbide layer 11 after about 10min, so that the damaged layer 14 can be removed together, and finally obtaining the whispering gallery microdisk resonator.
Comparing the optical quality factor of the whispering gallery micro-disc resonant cavity formed by directly etching silicon carbide by using focused ion beams and the optical quality factor of the whispering gallery micro-disc resonant cavity formed by using the preparation method provided by the application, please refer to fig. 4, wherein a curve 1 in fig. 4 is an optical transmission curve of the whispering gallery micro-disc resonant cavity formed by directly etching silicon carbide by using the focused ion beams, and a curve 2 is a transmission curve of the whispering gallery micro-disc resonant cavity formed by using the focused ion beam etching combined with the annealing oxidation method provided by the application; it can be seen that the curve 1 does not measure an obvious optical resonance peak, which indicates that the transmission loss of light in the structure is extremely large, and the curve 2 measures an optical resonance peak and the optical quality factor is 10200, which indicates that the preparation method provided by the application can effectively remove the damage layer caused by the ion beam to the material.
The above description is only exemplary of the present application and should not be taken as limiting the present application, as any modification, equivalent replacement, or improvement made within the spirit and principle of the present application should be included in the protection scope of the present application.

Claims (10)

1. A preparation method of an optical micro-nano structure is characterized by comprising the following steps:
obtaining a heterogeneous composite substrate; the heterogeneous composite substrate sequentially comprises a thin film layer, an insulating layer and a supporting substrate from top to bottom; the thin film layer is made of silicon material;
carrying out ion beam cutting on the heterogeneous composite substrate to obtain an optical micro-nano structure; the optical micro-nano structure comprises a damaged layer caused by ion beam cutting, and the damaged layer is positioned on the thin film layer;
annealing the optical micro-nano structure to form a silicon dioxide layer at the position of the damaged layer; the thickness of the silicon dioxide layer is larger than that of the damage layer;
and removing the silicon dioxide layer to remove the damaged layer together to obtain the undamaged optical micro-nano structure.
2. The method of claim 1, wherein after the obtaining the heterogeneous composite substrate and before the ion beam cutting the heterogeneous composite substrate, further comprising:
and forming a protective layer on the surface of the thin film layer.
3. The method according to claim 2, wherein after the ion beam cutting of the heterogeneous composite substrate and before the annealing of the optical micro-nano structure, the method further comprises:
and placing the heterogeneous composite substrate and the protective layer after the ion beam cutting into an etching solution to remove the protective layer.
4. The method of claim 3, wherein the protective layer is made of a metallic material;
the metal material includes at least one of chromium, nickel, titanium, and gold.
5. The method of claim 3, wherein the protective layer is made of a non-metallic material;
the non-metallic material comprises at least one of silicon oxide, silicon nitride, titanium oxide and aluminum oxide.
6. The method of claim 1, wherein the silicon material is silicon or silicon carbide.
7. The method according to claim 1, wherein the ion beam is any one of a gallium ion beam, a silicon ion beam, a helium ion beam, and a boron ion beam;
the energy of the ion beam is 1-100 keV; the beam current of the ion beam is 0.1 pA-100 nA.
8. The method of claim 1, wherein the annealing temperature is in a range of 200 to 1300 degrees celsius;
the annealing atmosphere is at least one of argon, nitrogen, oxygen and atmospheric atmosphere.
9. The method of claim 3, wherein the etching solution comprises hydrofluoric acid or a buffered oxide etch.
10. The method according to claim 1, wherein the optical micro-nano structure is any one of a micro-ring, a micro-disk, an optical waveguide and a photonic crystal.
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