CN114755761B - Preparation method of lithium niobate thin film submicron line width ridge type optical waveguide based on chromium mask - Google Patents
Preparation method of lithium niobate thin film submicron line width ridge type optical waveguide based on chromium mask Download PDFInfo
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/10—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type
- G02B6/12—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type of the integrated circuit kind
- G02B6/13—Integrated optical circuits characterised by the manufacturing method
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/10—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type
- G02B6/12—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type of the integrated circuit kind
- G02B6/122—Basic optical elements, e.g. light-guiding paths
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/10—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type
- G02B6/12—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type of the integrated circuit kind
- G02B6/13—Integrated optical circuits characterised by the manufacturing method
- G02B6/132—Integrated optical circuits characterised by the manufacturing method by deposition of thin films
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/10—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type
- G02B6/12—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type of the integrated circuit kind
- G02B6/13—Integrated optical circuits characterised by the manufacturing method
- G02B6/136—Integrated optical circuits characterised by the manufacturing method by etching
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/20—Exposure; Apparatus therefor
- G03F7/2051—Exposure without an original mask, e.g. using a programmed deflection of a point source, by scanning, by drawing with a light beam, using an addressed light or corpuscular source
- G03F7/2059—Exposure without an original mask, e.g. using a programmed deflection of a point source, by scanning, by drawing with a light beam, using an addressed light or corpuscular source using a scanning corpuscular radiation beam, e.g. an electron beam
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/10—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type
- G02B6/12—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type of the integrated circuit kind
- G02B2006/12035—Materials
- G02B2006/1204—Lithium niobate (LiNbO3)
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Abstract
The invention discloses a preparation method of a lithium niobate thin film submicron line width ridge type optical waveguide based on a chromium mask, which comprises the following steps: obtaining a lithium niobate film sample to be processed; depositing an aluminum film on the surface of the lithium niobate thin film sample by using an electron beam evaporation coating system, coating photoresist on the surface of the aluminum film in a spinning mode, and etching a mask pattern on the sample by using an electron beam exposure photoetching machine; placing the sample in a developing solution for developing, and depositing a chromium film on the surface of the sample by using an electron beam evaporation coating system; putting the sample into stripping liquid, removing the photoresist and leaving a chromium mask pattern; and etching the sample by using the inductively coupled plasma to obtain the lithium niobate thin film submicron line width ridge type optical waveguide. The method can prepare the ridge type optical waveguide with the submicron line width, the side wall of the optical waveguide is high in verticality, and the lithium niobate optical waveguide device processed based on the process is small in size, easy to integrate and good in optical constraint condition.
Description
Technical Field
The invention belongs to the technical field of micro-nano photonic device processing, and particularly relates to a preparation method of a lithium niobate thin film submicron line width ridge type optical waveguide.
Background
Lithium niobate (LiNbO) 3 LN) is an important optical crystal material, and has a wide application in the field of optoelectronics. The existing preparation method of the mature lithium niobate optical waveguide mainly adopts a proton exchange method and a titanium diffusion method to prepare the optical waveguide on the lithium niobate crystal, and the optical waveguide prepared by the method has wider linewidth, so that the device has the problems of large volume and difficult integration. The method for manufacturing the optical waveguide on the monocrystal lithium niobate film by photoetching and etching becomes a research hotspot in recent years, and the method can be used for processing an optical waveguide device with narrower line width and smaller size, and can also provide better optical constraint conditions to obtain the optical waveguide device with easier integration and better performance.
Disclosure of Invention
The invention provides a preparation method of a lithium niobate thin film submicron line width ridge type optical waveguide based on a chromium mask, wherein the line width of the optical waveguide processed by the process flows of electron beam evaporation coating, electron beam exposure lithography, inductive coupling plasma etching and the like can reach submicron level, and the inclination angle of the side wall of the waveguide can reach 71 degrees. The invention specifically adopts the following technical scheme:
a preparation method of a lithium niobate thin film submicron line width ridge type optical waveguide based on a chromium mask comprises the following steps:
s1, obtaining a lithium niobate thin film sample to be processed, wherein the lithium niobate thin film comprises a lithium niobate layer, a silicon dioxide layer and a silicon substrate, the thickness of the lithium niobate layer is 600nm, the thickness of the silicon dioxide layer is 4 mu m, and the thickness of the silicon substrate is about 0.5mm;
s2, cleaning and drying the lithium niobate thin film sample;
s3, depositing an aluminum film on the surface of the lithium niobate thin film sample by using an electron beam evaporation coating system, wherein the thickness of the aluminum film is 10-20 nm;
s4, spin-coating a photoresist on the surface of the aluminum film, wherein the type of the photoresist is electron beam positive photoresist UV135, the spin-coating rotation speed is 3000r/min, and the spin-coating time is 1min;
s5, drying the sample obtained in the step S4, and drying for 1min at 130 ℃;
s6, etching a mask pattern on the sample obtained in the step S5 by using an electron beam exposure photoetching machine;
s7, after photoetching exposure is finished, drying the sample for 1.5min at 130 ℃;
s8, placing the sample in MF319 developing solution for developing for 1.5min;
s9, depositing a chromium film on the surface of the sample by using an electron beam evaporation coating system, wherein the beam current is 40-100 mA, the coating speed is controlled to be 0.05-0.1 nm/S, and the thickness of the chromium film is 150nm;
s10, placing the sample into stripping liquid, removing the photoresist, and leaving a chromium mask pattern;
s11, etching a sample by using inductively coupled plasma, wherein the etching gas is argon and perfluorobutene, the flow rate is 20-25 sccm, the radio frequency power is 50-250W, and the etching rate of lithium niobate is 30-60 nm/min;
and S12, cleaning a chromium mask and an aluminum film remained on the sample by adopting a chromium etching solution to obtain the lithium niobate thin film submicron line width ridge type optical waveguide.
Furthermore, the lithium niobate thin film submicron line width ridge type optical waveguide has a line width of 0.6-1.5 μm, a depth of 200-500 nm and a side wall inclination angle of 64-71 degrees.
Further, the step S2 specifically comprises the steps of putting a lithium niobate thin film sample into an acetone solution for ultrasonic treatment for 3-5 min, taking out the sample, flushing the sample for 10-20S under deionized water, and blowing the sample on dust-free paper to blow dry surface moisture by air; placing on a hot plate, and baking at 100 deg.C for 1min.
Further, in the step S10, the stripping solution is acetone, isopropanol or absolute ethyl alcohol.
Further, in the step S12, the sample is placed in the chromium etching solution for 10min.
The invention has the beneficial effects that:
(1) The invention adopts the electron beam exposure photoetching method, so that the mask pattern can have submicron-level line width, and the lithium niobate optical waveguide device processed based on the process has small volume, easy integration and good optical constraint condition.
(2) Lithium niobate is a non-conductive material, and when electron beam exposure lithography is performed, surface charge accumulation can be caused by non-conductivity of the sample surface, so that the exposure effect is influenced. The method usually adopts a method of adding a surface charge remover during photoresist leveling, the cost of the surface charge remover is high, and all photoresists are not provided with the applicable surface charge remover. According to the invention, the surface of the sample is conductive by plating a layer of 10-20 nm aluminum film on the surface of the lithium niobate thin film sample, so that the electron beam exposure photoetching effect is improved, and the subsequent etching effect cannot be influenced by the aluminum film with the thickness.
(3) The method adopts the method of firstly photoetching and then plating the metal chromium film to manufacture the chromium etching mask, and compared with the method of adopting the photoresist mask to etch the chromium film to obtain the chromium mask, the method adopts the electron beam evaporation to more easily control the appearance of the chromium mask; the chromium is used as a mask material, and has higher etching selection ratio compared with a silicon oxide mask or a photoresist mask, so that a better etching effect is obtained.
(4) According to the invention, argon and perfluorobutene are selected as etching gases, and process parameters after optimization are combined, so that compared with the traditional argon ion reaction etching, the etching selectivity is higher, and the verticality of the side wall of the optical waveguide is higher.
Drawings
In order to illustrate embodiments of the present invention or technical solutions in the prior art more clearly, the drawings that are needed in the embodiments will be briefly described below, so that the features and advantages of the present invention can be understood more clearly by referring to the drawings, which are schematic and should not be construed as limiting the present invention in any way, and other drawings can be obtained by those skilled in the art without inventive effort. Wherein:
FIG. 1 is a process flow diagram, which is to complete the processing of lithium niobate thin film optical waveguide by processes of electron beam evaporation aluminum plating, glue homogenizing, electron beam exposure, development, electron beam evaporation chromium plating, mask stripping, inductively coupled plasma etching, chromium removal, aluminum and the like in sequence.
FIG. 2 is a three-dimensional scanning image of lithium niobate thin film optical waveguide under atomic force microscope, the waveguide width is 1 μm, the waveguide depth is 200nm, and the side wall inclination angle is 64 °.
FIG. 3 is a three-dimensional scanning image of lithium niobate thin film optical waveguide under atomic force microscope, the waveguide width is 1 μm, the waveguide depth is 292nm, and the sidewall inclination angle is 71 °.
Detailed Description
In order that the above objects, features and advantages of the present invention can be more clearly understood, a more particular description of the invention, taken in conjunction with the accompanying drawings and detailed description, is set forth below. It should be noted that the embodiments of the present invention and features of the embodiments may be combined with each other without conflict.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, however, the present invention may be practiced in other ways than those specifically described herein, and therefore the scope of the present invention is not limited by the specific embodiments disclosed below.
Example 1
The invention provides a preparation method of a lithium niobate thin film submicron line width ridge type optical waveguide, and figure 1 is a process flow chart, and the specific process steps, process parameters and operation details are as follows:
the method comprises the following steps: and obtaining a lithium niobate thin film sample to be processed, wherein the lithium niobate thin film comprises a lithium niobate layer, a silicon dioxide layer and a silicon substrate.
Step two: the sample was washed and dried. Putting a lithium niobate thin film sample into an acetone solution for ultrasonic treatment for 3-5 min, then taking out the sample, flushing the sample under deionized water for 10-20 s, and then putting the sample on dust-free paper to blow dry surface moisture by air blowing; the lithium niobate thin film sample was placed on a hot plate and baked at 100 ℃ for 1min.
Step three: electron beam evaporation of the aluminized film. And depositing an aluminum film with the thickness of 20nm on the surface of the sample by using an electron beam evaporation coating system.
Step four: and (6) glue homogenizing. The lithium niobate film is placed in the center of a vacuum adsorption disc of a spin coater, and the rotating speed is 3000r/min and the acceleration is 1000r/min/s. And after vacuum adsorption, starting rotation, dripping 3-5 drops of UV135 photoresist at the center of the sample after 3-5 seconds, stopping rotation after 55 seconds, closing vacuum adsorption, and taking down the sample.
Step five: and (6) pre-baking. The sample was placed on a hot plate and baked at 130 ℃ for 1min.
Step six: and (4) electron beam exposure lithography. And etching a mask pattern on the lithium niobate thin film sample after photoresist homogenizing by using an electron beam exposure photoetching machine.
Step seven: and (5) postbaking. After the photolithographic exposure was completed, the sample was taken out and placed on a hot plate, and baked at 130 ℃ for 1.5min.
Step eight: and (6) developing. Soaking the sample in a developing solution for 1.5min, taking the sample out of the developing solution, flushing the sample in deionized water for 1min under the condition that the surface is covered by the developing solution, and then placing the sample on dust-free paper to blow the surface moisture by air blowing.
Step nine: and (4) performing electron beam evaporation chromium plating. Depositing a chromium film with the thickness of 150nm on the surface of the sample by using an electron beam evaporation coating system.
Step ten: and stripping the mask. And (3) putting the sample on a stripping frame upside down, immersing the sample in an acetone solution, carrying out ultrasonic treatment for 1min, taking out the sample, carrying out ultrasonic treatment for 1min by changing the clean acetone solution, then flushing the sample with deionized water for 30s, and then putting the sample on dust-free paper and drying the surface moisture of the dust-free paper.
Step eleven: and (4) etching by inductively coupled plasma. Argon and perfluorobutene are used as etching gases, the gas flow rate is 22.5sccm, the radio frequency power is 100W, the etching selection ratio of lithium niobate to chromium is 5.1: 1, the etching rate of lithium niobate is 40nm/min, and the etching time is 5min.
Step twelve: and removing the chromium mask. And (3) putting the sample in a chromium etching solution for 10min, dissolving the rest chromium and aluminum, taking out the sample, washing the sample under deionized water for 1min, and then putting the sample on dust-free paper to blow and dry surface moisture by the dust-free paper.
The processed lithium niobate thin film optical waveguide is characterized under an atomic force microscope, and fig. 2 is a three-dimensional scanning diagram of the lithium niobate thin film optical waveguide under the atomic force microscope in the example, and the obtained waveguide line width is 1 μm, the waveguide depth is 200nm, and the side wall inclination angle is 64 degrees.
Example 2
The invention provides a preparation method of a lithium niobate thin film submicron line width ridge type optical waveguide, and figure 1 is a process flow chart, and the specific process steps, process parameters and operation details are as follows:
the method comprises the following steps: and obtaining a lithium niobate thin film sample to be processed, wherein the lithium niobate thin film comprises a lithium niobate layer, a silicon dioxide layer and a silicon substrate.
Step two: the samples were washed and dried. Putting a lithium niobate thin film sample into an acetone solution for ultrasonic treatment for 3-5 min, then taking out the sample, flushing the sample under deionized water for 10-20 s, and then putting the sample on dust-free paper to blow dry surface moisture by air blowing; the lithium niobate thin film sample was placed on a hot plate and baked at 100 ℃ for 1min.
Step three: electron beam evaporation of the aluminized film. And depositing an aluminum film with the thickness of 10nm on the surface of the sample by using an electron beam evaporation coating system.
Step four: and (6) glue homogenizing. The lithium niobate film is placed in the center of a vacuum adsorption disc of a spin coater, and the rotating speed is 3000r/min and the acceleration is 1000r/min/s. And after vacuum adsorption, starting rotation, dripping 3-5 drops of UV135 photoresist at the center of the sample after 3-5 seconds, stopping rotation after 55 seconds, closing vacuum adsorption, and taking down the sample.
Step five: and (6) pre-baking. The sample was placed on a hot plate and baked at 130 ℃ for 1min.
Step six: and (4) electron beam exposure lithography. And etching a mask pattern on the lithium niobate thin film sample after photoresist homogenizing by using an electron beam exposure photoetching machine.
Step seven: and (5) postbaking. After the photolithographic exposure was completed, the sample was taken out and placed on a hot plate, and baked at 130 ℃ for 1.5min.
Step eight: and (5) developing. Soaking the sample in a developing solution for 1.5min, taking the sample out of the developing solution, flushing the sample in deionized water for 1min under the condition that the surface is covered by the developing solution, and then placing the sample on dust-free paper to blow the surface moisture by air blowing.
Step nine: and (4) performing electron beam evaporation chromium plating. Depositing a chromium film with the thickness of 150nm on the surface of the sample by using an electron beam evaporation coating system.
Step ten: and stripping the mask. And (3) putting the sample on a stripping frame upside down, immersing the sample in an acetone solution, carrying out ultrasonic treatment for 1min, taking out the sample, carrying out ultrasonic treatment for 1min by changing the clean acetone solution, then flushing the sample with deionized water for 30s, and then putting the sample on dust-free paper and drying the surface moisture of the dust-free paper.
Step eleven: and (4) etching by inductively coupled plasma. Argon and perfluorobutene are used as etching gases, the gas flow rate is 22.5sccm, the radio frequency power is 200W, the etching selection ratio of lithium niobate to chromium is 5.6: 1, the etching rate of lithium niobate is 58.4nm/min, and the etching time is 5min.
Step twelve: and removing the chromium mask. And (3) putting the sample in a chromium etching solution for 10min, dissolving the residual chromium and aluminum, taking out the sample, rinsing the sample under deionized water for 1min, and then putting the sample on dust-free paper to blow and dry surface moisture by the dust-free paper.
The processed lithium niobate thin film optical waveguide is characterized under an atomic force microscope, fig. 3 is a three-dimensional scanning diagram of the lithium niobate thin film optical waveguide under the atomic force microscope in the example, and the obtained waveguide line width is 1 μm, the ridge waveguide depth is 292nm, and the side wall inclination angle is 71 degrees.
Claims (5)
1. A preparation method of a lithium niobate thin film submicron line width ridge type optical waveguide based on a chromium mask is characterized by comprising the following steps:
s1, obtaining a lithium niobate thin film sample to be processed, wherein the lithium niobate thin film comprises a lithium niobate layer, a silicon dioxide layer and a silicon substrate, the thickness of the lithium niobate layer is 600nm, the thickness of the silicon dioxide layer is 4 microns, and the thickness of the silicon substrate is 0.5mm;
s2, cleaning and drying the lithium niobate thin film sample;
s3, depositing an aluminum film on the surface of the lithium niobate thin film sample by using an electron beam evaporation coating system, wherein the thickness of the aluminum film is 10-20 nm;
s4, spin-coating a photoresist on the surface of the aluminum film, wherein the type of the photoresist is electron beam positive photoresist UV135, the spin-coating rotation speed is 3000r/min, and the spin-coating time is 1min;
s5, drying the sample obtained in the step S4, and drying for 1min at 130 ℃;
s6, etching a mask pattern on the sample obtained in the step S5 by using an electron beam exposure photoetching machine;
s7, after photoetching exposure is finished, drying the sample for 1.5min at 130 ℃;
s8, placing the sample in MF319 developing solution for developing for 1.5min;
s9, depositing a chromium film on the surface of the sample by using an electron beam evaporation coating system, wherein the beam current is 40-100 mA, the coating speed is controlled within the range of 0.05-0.1 nm/S, and the thickness of the chromium film is 150nm;
s10, placing the sample into stripping liquid, removing the photoresist, and leaving a chromium mask pattern;
s11, etching a sample by using inductively coupled plasma, wherein the etching gas is argon and perfluorobutene, the flow rate is 20-25 sccm, the radio frequency power is 50-250W, and the etching rate of lithium niobate is 30-60 nm/min;
and S12, cleaning the residual chromium mask and the aluminum film on the sample by adopting a chromium etching solution to obtain the lithium niobate thin film submicron line width ridge type optical waveguide.
2. The method for preparing the submicron linewidth ridge-type optical waveguide of the lithium niobate thin film based on the chrome mask as claimed in claim 1, wherein the submicron linewidth ridge-type optical waveguide of the lithium niobate thin film has a linewidth of 0.6-1.5 μm, a depth of 200-500 nm, and a sidewall inclination angle of 64-71 °.
3. The method for preparing a submicron-linewidth ridge-type optical waveguide of a lithium niobate thin film based on a chromium mask as claimed in claim 1, wherein the step S2 specifically comprises the steps of placing a lithium niobate thin film sample into an acetone solution for ultrasonic treatment for 3-5 min, taking out the sample, flushing the sample under deionized water for 10-20S, and placing the sample on dust-free paper to blow dry surface moisture by air blowing; placing on a hot plate, and baking at 100 deg.C for 1min.
4. The method for preparing a submicron-linewidth ridge-type optical waveguide of lithium niobate thin film based on chrome mask as claimed in claim 1, wherein in step S10, the stripping solution is acetone or isopropanol or absolute ethyl alcohol.
5. The method for preparing a submicron line width ridge type optical waveguide of lithium niobate thin film based on chrome mask as claimed in claim 1, wherein in step S12, the sample is placed in a chrome etching solution for 10min.
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| CN116299857B (en) * | 2023-02-09 | 2024-05-07 | 江苏浦丹光电技术有限公司 | Lithium niobate thin film optical waveguide and preparation method thereof |
| CN116931367B (en) * | 2023-09-18 | 2024-01-19 | 济南量子技术研究院 | Lithium niobate thin film ridge waveguide modulator and preparation method thereof |
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