CN115598755A - Manufacturing method of high-refractive-index helical tooth grating - Google Patents

Manufacturing method of high-refractive-index helical tooth grating Download PDF

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CN115598755A
CN115598755A CN202211386284.3A CN202211386284A CN115598755A CN 115598755 A CN115598755 A CN 115598755A CN 202211386284 A CN202211386284 A CN 202211386284A CN 115598755 A CN115598755 A CN 115598755A
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Prior art keywords
imprinting
grating
pattern
helical
seed layer
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崔波
严正
李金涛
潘艾希
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Hangzhou Detective Nano Technology Co ltd
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Hangzhou Detective Nano Technology Co ltd
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    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/18—Diffraction gratings
    • G02B5/1847—Manufacturing methods
    • 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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C23C14/083—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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/10—Glass or silica
    • 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
    • C23C14/225—Oblique incidence of vaporised material on substrate
    • 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
    • C23C14/24—Vacuum evaporation
    • C23C14/28—Vacuum evaporation by wave energy or particle radiation
    • C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/18—Diffraction gratings
    • G02B5/1847—Manufacturing methods
    • G02B5/1857—Manufacturing methods using exposure or etching means, e.g. holography, photolithography, exposure to electron or ion beams

Abstract

The invention provides a method for manufacturing a high-refractive-index helical tooth grating, which comprises the following steps: s1, forming a seed layer pattern on a grating substrate, wherein the seed layer pattern is a plurality of lines arranged at periodic intervals; and S2, depositing a layer of helical grating structure material on the seed layer pattern by utilizing a glancing angle deposition technology. The present invention uses GLAD angle deposition (GLAD) for the fabrication of high index helical gratings.

Description

Manufacturing method of high-refractive-index helical tooth grating
Technical Field
The invention belongs to the technical field of optical elements, and particularly relates to a manufacturing method of a high-refractive-index helical tooth grating.
Background
A skewed tooth grating is a high performance optical element with a periodic spatial structure. Since a helical grating is generally highly efficient at a particular diffraction order, its primary function is to couple light into the optical waveguide. The excellent optical performance of the helical tooth grating makes it widely used in aerospace, telecommunications, spectroscopy, and the current rapidly developing Virtual Reality (VR) and Augmented Reality (AR) fields. High index helical gratings, which provide a larger viewing angle, are important components in AR glasses.
The existing method for manufacturing the helical grating comprises the steps of performing reactive ion etching by using a Faraday cage and realizing the helical grating structure by using ion beam etching and reactive ion beam etching. The Faraday cage is used for reactive ion etching, and the Faraday cage is only suitable for batch processing of the helical tooth grating in a small range. The ion beam etching and the reactive ion beam etching can be combined to realize the processing of the skewed tooth grating structure in a large range, but the operation is complex. These two methods for manufacturing the skewed tooth grating are widely used in manufacturing the grating made of the conventional material such as silica (n = 1.5) skewed tooth grating, but are difficult to be applied to some high refractive index materials due to the limitation of the etching method.
The nano-imprint method proposed in recent years has mass-produced a high-refractive-index helical grating by filling a resin with nanoparticles of a high-refractive-index material such as titanium dioxide (TiO 2). Mass production is achieved by the nanoimprint method. However, in this scheme, the degree of nanoparticle filling needs to be strictly controlled, the imprint template has a corresponding service life, and certain defects may exist in the pattern transfer process.
Disclosure of Invention
The invention aims to solve the following technical problems: in the prior art, the method for manufacturing the helical tooth grating by using the Faraday cage to perform reactive ion etching and using the ion beam etching and the reactive ion beam etching to realize the helical tooth grating structure is difficult to apply to certain high-refractive-index materials, the nanoparticle filling degree of the method for manufacturing the helical tooth grating with the high-refractive-index helical tooth grating structure by using the nano imprinting method needs to be strictly controlled, the imprinting template has corresponding service life, and certain defects may exist in the pattern transfer process.
The invention provides a manufacturing method of a high-refractive-index helical tooth grating, which can avoid various technical problems caused by etching of corresponding materials.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method of manufacturing a high index grating comprising:
s1, forming a seed layer pattern on a grating substrate, wherein the seed layer pattern is a plurality of lines periodically arranged at intervals;
and S2, depositing a layer of helical grating structure material on the seed layer pattern by utilizing a glancing angle deposition technology.
As a preferred technical solution, step S1 specifically includes:
a101, spin-coating a layer of electron beam resist on a grating substrate;
a102, forming a design pattern on the electron beam resist layer by using electron beam exposure;
a103, developing at room temperature after exposure is finished;
a104, transferring the design pattern on the electron beam resist layer to a grating substrate by using reactive ion etching to form a seed layer pattern;
and a105, removing the residual electron beam resist by using plasma.
As a preferred technical solution, step S1 specifically includes:
b101, spin-coating a layer of imprinting material on the grating substrate;
b102, performing nano-imprinting on an imprinting material by using an imprinting template to form a plurality of lines arranged at intervals in a period;
b103, removing the imprinting material by using plasma until the imprinting material between the lines is removed, so as to obtain an imprinting pattern;
b104, transferring the design pattern on the imprinting pattern to a grating substrate by utilizing reactive ion etching to form a seed layer pattern;
and b105, removing residual imprinting materials by using plasma.
As a preferred technical solution, step S1 specifically includes:
c101, spin-coating a layer of imprinting material on the grating substrate;
c102, performing nano-imprinting on the imprinting material by using the imprinting template to form a plurality of lines arranged at intervals in a period;
and c103, removing the imprinting material by using plasma until the imprinting material between the lines is removed, so as to obtain the seed layer pattern.
As a preferred technical scheme, quartz glass is selected as a grating substrate, ZEP520A diluted by anisole 1 2 As the material of the helical grating structure.
As a preferred technical scheme, quartz glass is selected as a grating substrate, polystyrene is selected as a stamping material, a hot nano-stamping method is adopted as a nano-stamping method, and HfO is selected 2 And SiO 2 As the material of the helical grating structure.
As a preferred technical scheme, polyethylene glycol terephthalate is selected as a grating substrate, the imprinting material is ultraviolet nano-imprinting glue, the nano-imprinting method is ultraviolet nano-imprinting, and TiO is selected 2 As the material of the helical grating structure.
After the technical scheme is adopted, the invention has the following advantages:
oblique Angle Deposition (GLAD), also known as grazing Angle Deposition, or large Angle Deposition. The method is generally used for preparing a film with controllable morphology (refer to the patent of optical glass micron-sized space debris protective film with the publication number of CN 106987804B) and a nanowire (refer to the patent of indium antimonide nanowire preparation and manganese doping method based on a multi-step glancing angle deposition method with the publication number of CN 105862122B).
The present invention uses a tilted angle deposition technique (GLAD) for the fabrication of high index grating. The method solves the technical problems that the method for manufacturing the helical tooth grating by using the Faraday cage to perform reactive ion etching and the method for manufacturing the helical tooth grating by using the ion beam etching and the reactive ion beam etching to realize the helical tooth grating structure are difficult to apply to certain high-refractive-index materials, the nanoparticle filling degree of the method for manufacturing the helical tooth grating with the high-refractive-index helical tooth grating structure by using the nano imprinting method needs to be strictly controlled, an imprinting template has corresponding service life, and certain defects may exist in the pattern transfer process. Meanwhile, because the corresponding evaporation material is directly used for deposition instead of nano-particle implantation, the process does not worry about influencing the scattering rate of the material.
The method provided by the invention can realize the manufacture of a plurality of repeated unit helical tooth grating structures on one wafer. Subsequently, a plurality of coupling-in units are separated out by means of chip dicing. The optical coupling function is achieved by integrating a single incoupling unit onto a wafer that has completed the processing of the outcoupling unit. The method can greatly improve the large-scale processing efficiency of the optical device.
Drawings
FIG. 1 is a flowchart illustrating a method for manufacturing a high refractive index grating according to a first embodiment;
FIG. 2 is a flowchart illustrating a method for fabricating a high refractive index grating according to a second embodiment;
FIG. 3 is a flowchart illustrating a method for fabricating a high-index grating according to a third embodiment;
in the figure:
1-quartz glass; 2-ZEP520A electron beam resist; 3-an electron beam; 4-TiO 2 2 A vapor deposition source; 5-evaporation dip angle; 6-inclined tooth grating inclination angle; 7-TiO 2 (ii) a 8-polystyrene; 9-hot nano-imprinting a template; 10-HfO 2 and SiO2; 11-HfO 2 and SiO2 vapor deposition sources; 12-a PET substrate; 13-ultraviolet nanoimprint glue; 14-ultraviolet nano-imprinting template; 15-UV.
Detailed Description
The present invention will be described in further detail with reference to the following drawings and specific examples.
Example one
As shown in FIG. 1, this example provides a method for manufacturing a high refractive index grating with helical teeth, and produces a TiO 2 (n = 2.3) skewed tooth grating.
The method comprises the following specific steps:
1. quartz glass 1 is selected as a substrate;
the quartz glass 1 contains SiO as a main component 2 ；
2. Spin-coating a layer of ZEP520A electron beam resist 2 on the surface of the substrate;
ZEP520A e-beam resist 2 was diluted with 1;
3. baking on a hot plate at 180 ℃ for 3 minutes;
4. as shown in FIG. 1a, the substrate is exposed by electron beam 3 at a dose of 150 μ C/cm 2 Forming a design pattern by exposure with an electron beam 3;
here, the ZEP520A electron beam resist 2 pattern size was 150nm wide with a period of 400nm;
5. as shown in fig. 1b, the sample is immersed in a ZED-N50 developing solution at room temperature for developing for 90 seconds, and after the development is finished, the sample is washed by isopropanol and dried;
6. the pattern in the resist was transferred to SiO under the following etching conditions 2 Layer of SiO 2 The height of the seed layer pattern is 30nm:
reactive ion etching conditions: 15sccm O2, 40ccm C4F8, 10 mTorr, 200W RF, 2500W ICP, 50 ℃;
7. as shown in fig. 1c, oxygen plasma was used to remove the residual ZEP520A resist;
8. as shown in fig. 1d, by means of a tilted angle deposition technique (GLAD) through TiO 2 Deposition source 4 deposition of TiO 2 7 above the seed layer;
in this example, the oblique angle deposition technique (GLAD) evaporates TiO by electron beam 2 The realization is that the dip angle of evaporation plating is 5 degrees at 85 degrees, and the TiO obtained by evaporation plating 2 The height of 7 is determined by the evaporation rate and the evaporation time.
By adopting the technical scheme, the TiO with the period of 400nm, the inclined tooth grating inclination angle 6 of about 55 degrees and the duty ratio of about 0.375 can be obtained 2 Skewed tooth grating structure. The implementation according to the embodiment can realize the batch preparation of the high-refractive-index helical tooth grating.
Example two
As shown in fig. 2, the present embodiment provides a method for manufacturing a high-refractive-index helical grating, which manufactures a mixture of HfO2 and SiO2 (n = 1.9) helical grating.
The method comprises the following specific steps:
1. quartz glass 1 is selected as a substrate;
2. as shown in fig. 2a, a layer of Polystyrene 8 (Polystyrene) was spin coated on the surface of the substrate, approximately 200nm thick;
3. as shown in fig. 2b, the hot nano-imprinting is performed using the prepared hot nano-imprinting stamp 9 under the following imprinting conditions: the temperature is 150 ℃, the pressure is 10bar, and the time is 3min;
4. cooling to 40 deg.C, and demolding to obtain the structure shown in FIG. 2 c;
5. oxygen plasma was used to remove the residual polystyrene resulting in a polystyrene pattern with a period of 200nm and a width of 50nm, as shown in FIG. 2 d;
6. as shown in FIG. 2e, the pattern in the resist was transferred to SiO under the following etch conditions 2 Layer of SiO 2 The seed layer pattern height was 30nm and the remaining polystyrene mask was removed:
reactive ion etching conditions: 15sccm O 2 、40ccm C 4 F 8 、10 mTorr、200W RF、2500W ICP、50°C；
7. As shown in fig. 2f, by using a tilted angle deposition technique (GLAD) through HfO 2 And SiO 2 Evaporation source 11 for depositing HfO 2 And SiO 2 10 above the seed layer;
in this embodiment, the oblique angle deposition (GLAD) technique is applied by simultaneous electron beam evaporation of HfO 2 And SiO 2 The realization is that the dip angle of evaporation plating is 80 degrees, the heights of HfO2 and SiO2 obtained by evaporation plating are determined by the evaporation plating rate and the evaporation plating time, the proportion is controlled by the respective evaporation plating rate, wherein the SiO2 is 2 The proportion is 14 percent.
By adopting the technical scheme, the HfO2 and SiO2 skewed tooth grating structure with the period of 200nm, the skewed tooth grating inclination angle of 6 degrees and the duty ratio of about 0.25 can be obtained. The implementation according to the embodiment can realize the batch preparation of the high-refractive-index helical tooth grating.
EXAMPLE III
As shown in fig. 3, this embodiment provides a method for manufacturing a high-refractive-index helical grating, which manufactures a TiO2 (n = 2.3) helical grating.
The method comprises the following specific steps:
1. selecting PET (polyethylene terephthalate) as a substrate;
2. as shown in FIG. 3a, a layer of ultraviolet nanoimprint resist 13 (PL-R-PC 1000) is spin coated on the surface of the PET substrate 12, and is about 200nm thick;
3. as shown in fig. 3b, UV nanoimprinting is performed by UV15 using the prepared UV nanoimprinting template 14 under the imprint conditions: the light intensity is 70mW/cm2, the pressure is 400kPa, and the time is 3min;
4. as shown in fig. 3d, demolding and removing residues by using oxygen-fluorine plasma to obtain a seed layer pattern;
the ultraviolet nanoimprint lithography glue 13 (PL-R-PC 1000) contains silicon, and during etching, fluorine-containing gas such as CF4 needs to be added into oxygen;
the size of the seed pattern is 100nm wide, the period is 200nm, and the height of the seed layer is 20nm;
5. as shown in fig. 3e, by means of a tilted angle deposition technique (GLAD) through TiO 2 Deposition source 4 deposition of TiO 2 7 above the seed layer;
in this example, the oblique angle deposition technique (GLAD) evaporates TiO by electron beam 2 The deposition inclination angle is 5 degrees and is 83 degrees, and the TiO obtained by deposition 2 Height 7 is determined by the evaporation rate and evaporation time.
By adopting the technical scheme, the TiO with the period of 200nm, the inclined tooth grating inclination angle of 6 about 52 degrees and the duty ratio of about 0.5 can be obtained 2 Skewed tooth grating structure. The implementation according to the embodiment can realize the batch preparation of the high-refractive-index helical tooth grating.
The finally formed grating structure, if some defects exist, can be repaired by subsequent processing such as annealing and the like.
The novel method for preparing the high-refractive-index helical-tooth grating, which combines electron beam lithography, oblique angle deposition and etching, can be applied to experimental research and development, but the electron beam exposure efficiency is low, and an advanced lithography technology is generally selected to replace electron beam exposure and applied to batch processing. The subsequent batch processing can be combined with the nanoimprint technology to realize large-scale batch production. .
The method provided by the invention can realize the manufacture of a plurality of repeated unit helical tooth grating structures on one wafer. Subsequently, a plurality of coupling-in units are separated out by means of chip dicing. The optical coupling function can be realized by integrating a single coupling-in unit on the wafer processed by the coupling-out unit. The method can greatly improve the large-scale processing efficiency of the optical device.
Other embodiments of the present invention than the preferred embodiments described above will be apparent to those skilled in the art from the present invention, and various changes and modifications can be made therein without departing from the spirit of the present invention as defined in the appended claims.

Claims (7)

1. A method of fabricating a high index grating comprising:
s1, forming a seed layer pattern on a grating substrate, wherein the seed layer pattern is a plurality of lines arranged at periodic intervals;
and S2, depositing a layer of helical grating structure material on the seed layer pattern by utilizing a glancing angle deposition technology.
2. The method according to claim 1, wherein the step S1 specifically comprises:
a101, spin-coating a layer of electron beam resist on a grating substrate;
a102, forming a design pattern on the electron beam resist layer by using electron beam exposure;
a103, developing at room temperature after exposure is finished;
a104, transferring the design pattern on the electron beam resist layer to a grating substrate by utilizing reactive ion etching to form a seed layer pattern;
and a105, removing the residual electron beam resist by using plasma.
3. The method for manufacturing a high refractive index helical grating according to claim 1, wherein the step S1 specifically comprises:
b101, spin-coating a layer of imprinting material on the grating substrate;
b102, carrying out nano-imprinting on an imprinting material by using an imprinting template to form a plurality of lines which are periodically arranged at intervals;
b103, removing the imprinting material by using plasma until the imprinting material between the lines is removed, so as to obtain an imprinting pattern;
b104, transferring the design pattern on the imprinting pattern to the grating substrate by utilizing reactive ion etching to form a seed layer pattern;
and b105, removing residual imprinting materials by using plasma.
4. The method according to claim 1, wherein the step S1 specifically comprises:
c101, spin-coating a layer of imprinting material on the grating substrate;
c102, performing nano-imprinting on the imprinting material by using the imprinting template to form a plurality of lines which are arranged at intervals in a period;
and c103, removing the imprinting material by using plasma until the imprinting material between the lines is removed, and obtaining the seed layer pattern.
5. The method according to claim 2, wherein quartz glass is used as the grating substrate, ZEP520A diluted with anisole 1 2 As the material of the helical grating structure.
6. The method as claimed in claim 3, wherein the grating substrate is quartz glass, the imprinting material is polystyrene, the nanoimprinting method is thermal nanoimprinting, and the HfO is selected 2 And SiO 2 As the material of the helical tooth grating structure.
7. The method of claim 4, wherein the grating substrate is polyethylene terephthalate, the imprinting material is UV nanoimprint resist, the nanoimprint method is UV nanoimprint, and TiO is used 2 As the material of the helical tooth grating structure.
CN202211386284.3A 2022-11-07 2022-11-07 Manufacturing method of high-refractive-index helical tooth grating Pending CN115598755A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202211386284.3A CN115598755A (en) 2022-11-07 2022-11-07 Manufacturing method of high-refractive-index helical tooth grating

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202211386284.3A CN115598755A (en) 2022-11-07 2022-11-07 Manufacturing method of high-refractive-index helical tooth grating

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Publication Number Publication Date
CN115598755A true CN115598755A (en) 2023-01-13

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