CN108288580B - Preparation method of optical biosensor based on one-dimensional photonic crystal coupling microcavity - Google Patents

Preparation method of optical biosensor based on one-dimensional photonic crystal coupling microcavity Download PDF

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CN108288580B
CN108288580B CN201710873280.0A CN201710873280A CN108288580B CN 108288580 B CN108288580 B CN 108288580B CN 201710873280 A CN201710873280 A CN 201710873280A CN 108288580 B CN108288580 B CN 108288580B
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soi
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CN108288580A (en
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王卓然
袁国慧
彭芳草
管磊
彭真明
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University of Electronic Science and Technology of China
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/027Making masks on semiconductor bodies for further photolithographic processing not provided for in group H01L21/18 or H01L21/34
    • GPHYSICS
    • G03PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03FPHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F7/00Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
    • G03F7/20Exposure; Apparatus therefor
    • G03F7/2022Multi-step exposure, e.g. hybrid; backside exposure; blanket exposure, e.g. for image reversal; edge exposure, e.g. for edge bead removal; corrective exposure
    • GPHYSICS
    • G03PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03FPHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F7/00Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
    • G03F7/26Processing photosensitive materials; Apparatus therefor
    • G03F7/38Treatment before imagewise removal, e.g. prebaking
    • GPHYSICS
    • G03PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03FPHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F7/00Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
    • G03F7/26Processing photosensitive materials; Apparatus therefor
    • G03F7/40Treatment after imagewise removal, e.g. baking

Abstract

The invention discloses a preparation method of an optical biosensor based on a one-dimensional photonic crystal coupling microcavity, which comprises the following steps: s1, cleaning the SOI sample; s2, placing the SOI sample in a thermostat with the temperature of 170-200 ℃ for baking for 2-5 min; s3, coating photoresist on the sample in a spin coating mode; s4, placing the sample in a thermostat with the temperature of 170-200 ℃ for drying for 10-15 min; s5, carrying out electron beam exposure on the sample, wherein the exposure pattern is a one-dimensional photonic crystal coupling micro-ring resonant cavity structure; s6, developing and fixing the exposed sample in sequence; s7, etching the sample by adopting ICP; and S8, washing the sample with a Piranha solution, washing with DI water, washing with an HF solution, and finally washing with DI water. The optical biosensor manufactured by the preparation method has the characteristics of high sensitivity, small detection limit, easy integration and the like, has simple requirements on equipment, is easy to realize in process, and is suitable for mass production.

Description

Preparation method of optical biosensor based on one-dimensional photonic crystal coupling microcavity
Technical Field
The invention belongs to the technical field of optical biosensor, and particularly relates to a preparation method of an optical biosensor based on a one-dimensional photonic crystal coupling microcavity.
Background
Biosensors currently used include electrochemical biosensors, optical biosensors, thermal biosensors, semiconductor biosensors, conductive/resistive biosensors, and acoustic wave biosensors, as detection mechanisms thereof. The optical biosensor has the advantages of lossless operation mode, electromagnetic interference resistance, high sensitivity, high-speed signal generation, high-speed reading rate and the like, has a very wide prospect, and is more and more widely concerned.
SOI optical biosensors are the research focus in the field, and most of the existing SOI-based optical biosensors use the evanescent wave detection principle, that is, a change in refractive index or concentration of a surrounding medium causes a change in the effective refractive index of a waveguide, and the change in the effective refractive index causes a shift in the optical spectrum. The concentration or refractive index information of the detected substance can be obtained by detecting the movement of the spectrum by the photoelectric detector. The preparation scheme becomes particularly critical in order to obtain SOI biosensors with excellent performance.
The experimental preparation of the SOI optical biosensor mainly comprises wet etching and dry etching. The wet etching is to shield the sample part exposed by the etching solution through a mask plate, and the required sensor structure is finally formed through the selective etching. In the wet etching process, the reaction of the etched sample and the etching solution is influenced by a plurality of factors, so that the etching process is not easy to control, and the width of the transverse etching is close to the depth of the vertical etching. Therefore, the fidelity of pattern etching is not ideal, and the minimum line width of the etched pattern is difficult to control. For dry Etching, the most common method is Plasma Etching (Plasma Etching). Compared with wet etching, the method has lower etching rate, but can well control the etching process. In addition, the verticality of the side wall of the optical waveguide is improved to some extent.
Therefore, how to prepare a high-performance biosensor with high sensitivity, small detection limit and easy integration by using an excellent process becomes a new research direction.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of an optical biosensor based on a one-dimensional photonic crystal coupling microcavity.
The purpose of the invention is realized by the following technical scheme: the preparation method of the optical biosensor based on the one-dimensional photonic crystal coupling microcavity comprises the following steps:
s1, preprocessing, and cleaning an SOI sample;
s2, pre-baking, namely placing the pretreated SOI sample in a thermostat at the temperature of 170-200 ℃ for baking for 2-5 min, and cooling to room temperature;
s3, gluing, namely coating photoresist on the sample subjected to the pre-baking treatment in a spin coating mode;
s4, post-baking, namely placing the sample after being coated with the glue in a thermostat at the temperature of 170-200 ℃ for baking for 10-15 min, and cooling to room temperature;
s5, exposure, wherein the sample after post-baking treatment is subjected to electron beam exposure, and the exposure pattern is a one-dimensional photonic crystal coupling micro-ring resonant cavity structure;
s6, developing and fixing, wherein the sample after exposure is sequentially subjected to developing and fixing operations and then cleaned by IPA solution;
s7, etching, namely etching the sample after the development and fixation treatment by adopting ICP (Inductively Coupled Plasma);
and S8, post-treatment, namely cleaning the etched sample by using a Piranha solution, then washing by using DI water, then cleaning by using an HF solution, and finally washing by using DI water.
Further, the step S1 specifically includes the following sub-steps:
s11, putting the SOI sample blown by nitrogen into an acetone solution, carrying out ultrasonic cleaning for 5-10 min, and then carrying out drying treatment, wherein the ultrasonic cleaning by the acetone solution is carried out to remove attachments on the surface of the SOI;
s12, putting the SOI sample processed in the step S11 into Piranha solution to be cleaned for 10-15 min, washing with DI water, and drying; the Piranha solution is prepared by mixing H at 150 deg.C2SO4And H2O2According to the following steps of 3: 1, and the Piranha solution is adopted to remove organic matters on the surface of the SOI;
s13, putting the SOI sample processed in the step S12 into an HF solution to be cleaned for 15-20S, removing oxide on the surface of the SOI, and drying the SOI sample after being washed by DI water;
further, the drying treatments in the steps S11, S12 and S13 are all drying with nitrogen.
Further, the specific implementation method of step S3 is as follows: spin-coating for 4-6 s at a rotation speed of 1000-1500 rpm, then spin-coating for 1-1.5 min at a rotation speed of 2000-3000 rpm, and blowing and sucking the SOI sample by using nitrogen in the spin-coating process. The photoresist is positive electron beam resist ZEP 520A.
Further, the specific implementation method in step S6 is: and developing the exposed sample in a ZED-N50 solvent for 1-1.5 min, and then fixing with MIBK for 30-60 s.
Further, in the step S7, the etching depth is 200-300 nm, and the used etching gas is SF6/C4F8
Further, in the step S8, the Piranha solution is used for cleaning for 10-15 min, and the HF solution is used for cleaning for 15-20S.
The invention has the beneficial effects that: according to the invention, firstly, attachments, oxides and organic matters on the surface of the SOI are removed by cleaning and dried, then, photoresist is coated on a sample subjected to pre-drying treatment by adopting a spin coating mode and dried, then, electron beam exposure and developing fixation of the one-dimensional photonic crystal coupling microcavity are carried out, and finally, the sample is etched and cleaned by ICP (inductively coupled plasma), so that the optical biosensor based on the one-dimensional photonic crystal coupling microcavity is obtained. The preparation method of the invention has simple requirements on equipment, is easy to realize in process, can reduce the manufacturing cost of manufacturing the optical biosensor, and is suitable for mass production.
Drawings
FIG. 1 is a flow chart of the preparation method of the optical biosensor based on the one-dimensional photonic crystal coupling microcavity of the present invention;
FIG. 2 is a schematic diagram of a SOI sample structure for use in the present invention;
FIG. 3 is a first structural diagram of an optical biosensor based on a one-dimensional photonic crystal coupled microcavity according to the present invention;
FIG. 4 is a structural diagram of a second optical biosensor based on a one-dimensional photonic crystal coupled microcavity according to the present invention;
description of reference numerals: 21. a silicon substrate; 22. a silicon oxide layer; 23. a silicon waveguide layer; 31. an input-output straight waveguide; 32. An output straight waveguide; 33. a coupling point; 34. a micro-ring resonant cavity; 401-402, 433-434, uniform round holes; 403-432, non-uniform circular holes.
Detailed Description
The technical scheme of the invention is further explained by combining the attached drawings.
As shown in fig. 1, the preparation method of the optical biosensor based on the one-dimensional photonic crystal coupling microcavity comprises the following steps:
s1, preprocessing, and cleaning an SOI sample;
s2, pre-baking, namely placing the pretreated SOI sample in a thermostat at the temperature of 170-200 ℃ for baking for 2-5 min, and cooling to room temperature;
s3, gluing, namely coating photoresist on the sample subjected to the pre-baking treatment in a spin coating mode;
s4, post-baking, namely placing the sample after being coated with the glue in a thermostat at the temperature of 170-200 ℃ for baking for 10-15 min, and cooling to room temperature;
s5, exposure, wherein the sample after post-baking treatment is subjected to electron beam exposure, and the exposure pattern is a one-dimensional photonic crystal coupling micro-ring resonant cavity structure;
s6, developing and fixing, wherein the sample after exposure is sequentially subjected to developing and fixing operations and then cleaned by IPA solution;
s7, etching, namely etching the sample after development and fixation treatment by adopting ICP (inductively coupled plasma);
and S8, post-treatment, namely cleaning the etched sample by using a Piranha solution, then washing by using DI water, then cleaning by using an HF solution, and finally washing by using DI water.
As shown in fig. 2, the SOI sample employed in the present invention is composed of a lower silicon substrate 21, an intermediate silicon oxide layer 22, and an upper silicon waveguide layer 23.
As shown in FIG. 3, the optical biosensor based on one-dimensional photonic crystal coupled microcavity prepared by the present invention comprises an input/output straight waveguide 31, an output straight waveguide 32 and a silicon-based micro-ring resonator 34. The input and output straight waveguides 31 and 32 are coupled with the micro-ring resonant cavity 34 to form a one-dimensional photonic crystal coupling microcavity. A plurality of non-uniform circular holes and a plurality of uniform circular holes are etched on the input-output straight waveguide 31. The non-uniform circular hole area and the uniform circular hole area are distributed in central symmetry about the coupling point 33 of the input-output straight waveguide 31 and the silicon-based micro-ring resonant cavity. The number of the non-uniform round holes is 2N, and N is 15.
As shown in FIG. 4, the non-uniform circular holes on the input-output straight waveguide 31 include non-uniform circular hole regions 403-432 and uniform circular hole regions 401-402, 433-434. The number of the non-uniform round holes is 30. The number of the uniform round holes is 4, and each side is distributed with 2. The non-uniform circular holes 417, 418 have a radius r 1416, 419 have a radius r 2415, 420 have a radius r 3414, 421 have a radius r 4413, 422 has a radius r 5412, 423 having a radius r 6411, 424 have a radius r 7410, 425 have a radius r 8409, 426 has a radius r 9408, 427 has a radius r 10407, 428 have a radius r 11406, 429 having a radius r12Radius of 405, 430 is r 13404, 431 have a radius r14The radius of the non-uniform circular holes 403, 432 is r15(ii) a Said r1>r2>…>r15
Figure RE-GDA0001688210200000041
(i ═ 1,2, …, 15). And r is1=0.1025um,r150.0725 um. The radius of the uniform circular holes 401-402, 433-434 is r160.0725um, and the period T of the one-dimensional photonic crystal is 0.325 um.
The technical solution of the present invention is further described below by specific examples to further show the operation procedures and advantages of the present invention.
Example 1
A preparation method of an optical biosensor based on a one-dimensional photonic crystal coupling microcavity comprises the following steps:
s1, preprocessing, and cleaning an SOI sample; the method specifically comprises the following substeps:
s11, putting the SOI sample blown by nitrogen into an acetone solution, cleaning for 5min by ultrasonic waves, and then drying by nitrogen, wherein the cleaning by the acetone solution and the ultrasonic waves is to remove attachments on the surface of the SOI;
s12, putting the SOI sample processed in the step S11 into Piranha solution to be cleaned for 10min, washing with DI water, and drying with nitrogen; the Piranha solution is prepared by mixing H at 150 deg.C2SO4And H2O2According to the following steps of 3: 1, and the Piranha solution is adopted to remove organic matters on the surface of the SOI;
s13, putting the SOI sample processed in the step S12 into an HF solution to be cleaned for 15S, removing oxide on the surface of the SOI, washing the SOI sample with DI water, and drying the SOI sample with nitrogen;
s2, pre-baking, namely placing the pretreated SOI sample in a thermostat with the temperature of 180 ℃ for baking for 2min, and cooling to room temperature;
s3, gluing, namely coating photoresist on the sample subjected to the pre-baking treatment in a spin coating mode; the specific implementation method comprises the following steps: spin-coating at 1500rpm for 5s, then at 3000rpm for 1.5min, and blowing nitrogen gas to suck SOI sample during spin-coating to obtain a coating with thickness of
Figure BDA0001417568440000051
The photoresist is positive electron beam resist ZEP 520A.
S4, post-baking, namely, placing the glued sample in a constant temperature oven at the temperature of 180 ℃ for baking for 10min, and cooling to room temperature;
s5, exposure, wherein the sample after post-baking treatment is subjected to electron beam exposure, the exposure pattern is a one-dimensional photonic crystal coupling micro-ring resonant cavity structure, and the waveguide width of the structure is 500 nm;
s6, developing and fixing, namely developing the exposed sample in a ZED-N50 solvent for 1min, fixing with MIBK for 30S, and cleaning with IPA solution;
s7, etching, namely etching the sample after development and fixation by adopting ICP (inductively coupled plasma), wherein the etching depth is 220nm, and the etching gas is SF6/C4F8
And S8, post-treatment, namely cleaning the etched sample for 10min by using a Piranha solution, then washing the sample by using DI water, then cleaning the sample for 15S by using an HF solution, and finally washing the sample by using DI water.
Example 2
A preparation method of an optical biosensor based on a one-dimensional photonic crystal coupling microcavity comprises the following steps:
s1, preprocessing, and cleaning an SOI sample; the method specifically comprises the following substeps:
s11, putting the SOI sample blown by nitrogen into an acetone solution, carrying out ultrasonic cleaning for 8min, and then carrying out drying treatment by nitrogen, wherein the ultrasonic cleaning by the acetone solution is carried out to remove attachments on the surface of the SOI;
s12, putting the SOI sample processed in the step S11 into Piranha solution to be cleaned for 12min, washing with DI water, and drying with nitrogen; the Piranha solution is prepared by mixing H at 150 deg.C2SO4And H2O2According to the following steps of 3: 1, and the Piranha solution is adopted to remove organic matters on the surface of the SOI;
s13, putting the SOI sample processed in the step S12 into an HF solution to be cleaned for 18S, removing oxide on the surface of the SOI, washing the SOI sample with DI water, and drying the SOI sample with nitrogen;
s2, pre-baking, namely placing the pretreated SOI sample in a thermostat with the temperature of 180 ℃ for 3min, and cooling to room temperature;
s3, coating glue, and adopting spin coatingCoating photoresist on the sample subjected to the pre-baking treatment; the specific implementation method comprises the following steps: spin-coating at 1500rpm for 5s, then at 2500rpm for 1.5min, and blowing nitrogen gas to suck SOI sample during spin-coating to obtain a coated layer with thickness of
Figure BDA0001417568440000061
The photoresist is positive electron beam resist ZEP 520A.
S4, post-baking, namely placing the glued sample in a constant temperature oven at the temperature of 180 ℃ for baking for 15min, and cooling to room temperature;
s5, exposure, wherein the sample after post-baking treatment is subjected to electron beam exposure, the exposure pattern is a one-dimensional photonic crystal coupling micro-ring resonant cavity structure, and the waveguide width of the structure is 500 nm;
s6, developing and fixing, wherein the sample after exposure treatment is developed in a ZED-N50 solvent for 1.2min, then fixed by MIBK for 45S, and then cleaned by IPA solution;
s7, etching the sample after development and fixation by adopting ICP, wherein the etching depth is 250nm, and the etching gas is SF6/C4F8
And S8, post-treatment, namely cleaning the etched sample for 12min by using a Piranha solution, then washing the sample by using DI water, then cleaning the sample for 18S by using an HF solution, and finally washing the sample by using DI water.
Example 3
A preparation method of an optical biosensor based on a one-dimensional photonic crystal coupling microcavity comprises the following steps:
s1, preprocessing, and cleaning an SOI sample; the method specifically comprises the following substeps:
s11, putting the SOI sample blown by nitrogen into an acetone solution, carrying out ultrasonic cleaning for 10min, and then carrying out drying treatment by nitrogen, wherein the ultrasonic cleaning by the acetone solution is carried out to remove attachments on the surface of the SOI;
s12, putting the SOI sample processed in the step S11 into Piranha solution for cleaning for 15min, washing with DI water, and drying with nitrogen;the Piranha solution is prepared by mixing H at 150 deg.C2SO4And H2O2According to the following steps of 3: 1, and the Piranha solution is adopted to remove organic matters on the surface of the SOI;
s13, putting the SOI sample processed in the step S12 into an HF solution to be cleaned for 20S, removing oxide on the surface of the SOI, washing the SOI sample with DI water, and drying the SOI sample with nitrogen;
s2, pre-baking, namely placing the pretreated SOI sample in a thermostat with the temperature of 180 ℃ for baking for 5min, and cooling to room temperature;
s3, gluing, namely coating photoresist on the sample subjected to the pre-baking treatment in a spin coating mode; the specific implementation method comprises the following steps: spin-coating at 1500rpm for 5s, then at 2000rpm for 1.5min, and blowing nitrogen gas to suck SOI sample during spin-coating to obtain a coating with thickness of
Figure BDA0001417568440000062
The photoresist is positive electron beam resist ZEP 520A.
S4, post-baking, namely, placing the glued sample in a thermostat with the temperature of 180 ℃ for baking for 12min, and cooling to room temperature;
s5, exposure, wherein the sample after post-baking treatment is subjected to electron beam exposure, the exposure pattern is a one-dimensional photonic crystal coupling micro-ring resonant cavity structure, and the waveguide width of the structure is 500 nm;
s6, developing and fixing, wherein the sample after exposure treatment is developed in a ZED-N50 solvent for 1.5min, then fixed by MIBK for 60S, and then cleaned by IPA solution;
s7, etching the sample after development and fixation by adopting ICP, wherein the etching depth is 200nm, and the etching gas is SF6/C4F8
And S8, post-treatment, namely cleaning the etched sample for 15min by using a Piranha solution, then washing the sample by using DI water, then cleaning the sample for 20S by using an HF solution, and finally washing the sample by using DI water.
Example 4
A preparation method of an optical biosensor based on a one-dimensional photonic crystal coupling microcavity comprises the following steps:
s1, preprocessing, and cleaning an SOI sample; the method specifically comprises the following substeps:
s11, putting the SOI sample blown by nitrogen into an acetone solution, carrying out ultrasonic cleaning for 7min, and then carrying out drying treatment by nitrogen, wherein the ultrasonic cleaning by the acetone solution is carried out to remove attachments on the surface of the SOI;
s12, putting the SOI sample processed in the step S11 into Piranha solution to be cleaned for 13min, washing with DI water, and drying with nitrogen; the Piranha solution is prepared by mixing H at 150 deg.C2SO4And H2O2According to the following steps of 3: 1, and the Piranha solution is adopted to remove organic matters on the surface of the SOI;
s13, putting the SOI sample processed in the step S12 into an HF solution to be cleaned for 17S, removing oxide on the surface of the SOI, washing the SOI sample with DI water, and drying the SOI sample with nitrogen;
s2, pre-baking, namely placing the pre-treated SOI sample in a thermostat with the temperature of 170 ℃ for baking for 5min, and cooling to room temperature;
s3, gluing, namely coating photoresist on the sample subjected to the pre-baking treatment in a spin coating mode; the specific implementation method comprises the following steps: spin coating is carried out for 6s at the rotating speed of 1000rpm, then spin coating is carried out for 1.5min at the rotating speed of 2000rpm, and nitrogen is used for blowing and sucking the SOI sample in the spin coating process, and the photoresist is positive electron beam resist ZEP 520A.
S4, post-baking, namely, placing the glued sample in a thermostat at the temperature of 170 ℃ for baking for 15min, and cooling to room temperature;
s5, exposure, wherein the sample after post-baking treatment is subjected to electron beam exposure, the exposure pattern is a one-dimensional photonic crystal coupling micro-ring resonant cavity structure, and the waveguide width of the structure is 500 nm;
s6, developing and fixing, wherein the exposed sample is developed in a ZED-N50 solvent for 1.3min, then fixed by MIBK for 50S, and then cleaned by IPA solution;
s7 etchingEtching the sample after development and fixation by ICP (inductively coupled plasma) with the etching depth of 300nm and the etching gas SF6/C4F8
And S8, post-treatment, namely cleaning the etched sample for 13min by using a Piranha solution, then washing the sample by using DI water, then cleaning the sample for 17S by using an HF solution, and finally washing the sample by using DI water.
Example 5
A preparation method of an optical biosensor based on a one-dimensional photonic crystal coupling microcavity comprises the following steps:
s1, preprocessing, and cleaning an SOI sample; the method specifically comprises the following substeps:
s11, putting the SOI sample blown by nitrogen into an acetone solution, cleaning for 5min by ultrasonic waves, and then drying by nitrogen, wherein the cleaning by the acetone solution and the ultrasonic waves is to remove attachments on the surface of the SOI;
s12, putting the SOI sample processed in the step S11 into Piranha solution to be cleaned for 10min, washing with DI water, and drying with nitrogen; the Piranha solution is prepared by mixing H at 150 deg.C2SO4And H2O2According to the following steps of 3: 1, and the Piranha solution is adopted to remove organic matters on the surface of the SOI;
s13, putting the SOI sample processed in the step S12 into an HF solution to be cleaned for 15S, removing oxide on the surface of the SOI, washing the SOI sample with DI water, and drying the SOI sample with nitrogen;
s2, pre-baking, namely placing the pretreated SOI sample in a thermostat with the temperature of 200 ℃ for baking for 2min, and cooling to room temperature;
s3, gluing, namely coating photoresist on the sample subjected to the pre-baking treatment in a spin coating mode; the specific implementation method comprises the following steps: spin-coat at 1200rpm for 4s, then at 3000rpm for 1.5min, and use nitrogen to blow and suck SOI sample during spin-coating, and the photoresist is positive electron beam resist ZEP 520A.
S4, post-baking, namely, placing the sample after being glued into a constant temperature oven at the temperature of 200 ℃ for baking for 10min, and then cooling to room temperature;
s5, exposure, wherein the sample after post-baking treatment is subjected to electron beam exposure, the exposure pattern is a one-dimensional photonic crystal coupling micro-ring resonant cavity structure, and the waveguide width of the structure is 500 nm;
s6, developing and fixing, namely developing the exposed sample in a ZED-N50 solvent for 1min, fixing with MIBK for 30S, and cleaning with IPA solution;
s7, etching the sample after development and fixation by adopting ICP, wherein the etching depth is 270nm, and the etching gas is SF6/C4F8
And S8, post-treatment, namely cleaning the etched sample for 10min by using a Piranha solution, then washing the sample by using DI water, then cleaning the sample for 15S by using an HF solution, and finally washing the sample by using DI water.
It will be appreciated by those of ordinary skill in the art that the embodiments described herein are intended to assist the reader in understanding the principles of the invention and are to be construed as being without limitation to such specifically recited embodiments and examples. Those skilled in the art can make various other specific changes and combinations based on the teachings of the present invention without departing from the spirit of the invention, and these changes and combinations are within the scope of the invention.

Claims (9)

1. The preparation method of the optical biosensor based on the one-dimensional photonic crystal coupling microcavity is characterized by comprising the following steps of: the method comprises the following steps:
s1, preprocessing, and cleaning an SOI sample; the method specifically comprises the following substeps:
s11, putting the SOI sample blown by nitrogen into an acetone solution, cleaning for 5-10 min by adopting ultrasonic waves, removing attachments on the surface of the SOI, and then drying;
s12, putting the SOI sample processed in the step S11 into Piranha solution to be cleaned for 10-15 min, removing organic matters on the surface of the SOI, then washing with DI water, and drying;
s13, putting the SOI sample processed in the step S12 into an HF solution to be cleaned for 15-20S, removing oxide on the surface of the SOI, and drying the SOI sample after being washed by DI water;
s2, pre-baking, namely placing the pretreated SOI sample in a thermostat at the temperature of 170-200 ℃ for baking for 2-5 min, and cooling to room temperature;
s3, gluing, namely coating photoresist on the sample subjected to the pre-baking treatment in a spin coating mode;
s4, post-baking, namely placing the sample after being coated with the glue in a thermostat at the temperature of 170-200 ℃ for baking for 10-15 min, and cooling to room temperature;
s5, exposure, wherein the sample after post-baking treatment is subjected to electron beam exposure, and the exposure pattern is a one-dimensional photonic crystal coupling micro-ring resonant cavity structure;
s6, developing and fixing, wherein the sample after exposure is sequentially subjected to developing and fixing operations and then cleaned by IPA solution;
s7, etching, namely etching the sample after development and fixation treatment by adopting ICP (inductively coupled plasma);
and S8, post-treatment, namely cleaning the etched sample by using a Piranha solution, then washing by using DI water, then cleaning by using an HF solution, and finally washing by using DI water.
2. The method for preparing an optical biosensor based on one-dimensional photonic crystal coupling microcavity as claimed in claim 1, wherein the method comprises the following steps: the SOI sample consists of a lower silicon substrate, a middle silicon oxide layer and an upper silicon waveguide layer.
3. The method for preparing an optical biosensor based on one-dimensional photonic crystal coupling microcavity as claimed in claim 1, wherein the method comprises the following steps: the Piranha solution is prepared by mixing H at 150 deg.C2SO4And H2O2According to the following steps of 3: 1, and mixing the components in a ratio of 1.
4. The method for preparing an optical biosensor based on one-dimensional photonic crystal coupling microcavity as claimed in claim 1, wherein the method comprises the following steps: the drying treatment in the steps S11, S12 and S13 is performed by using nitrogen.
5. The method for preparing an optical biosensor based on one-dimensional photonic crystal coupling microcavity as claimed in claim 1, wherein the method comprises the following steps: the specific implementation method of the step S3 is as follows: spin-coating for 4-6 s at the rotating speed of 1000-1500 rpm, then spin-coating for 1-1.5 min at the rotating speed of 2000-3000 rpm, and blowing and sucking the SOI sample by using nitrogen in the spin-coating process.
6. The method for preparing an optical biosensor based on one-dimensional photonic crystal coupling microcavity as claimed in claim 1 or 5, wherein the method comprises the following steps: the photoresist is positive electron beam resist ZEP 520A.
7. The method for preparing an optical biosensor based on one-dimensional photonic crystal coupling microcavity as claimed in claim 1, wherein the method comprises the following steps: the specific implementation method in step S6 is as follows: and developing the exposed sample in a ZED-N50 solvent for 1-1.5 min, and then fixing with MIBK for 30-60 s.
8. The method for preparing an optical biosensor based on one-dimensional photonic crystal coupling microcavity as claimed in claim 1, wherein the method comprises the following steps: in the step S7, the etching depth is 200-300 nm, and the etching gas is SF6/C4F8
9. The method for preparing an optical biosensor based on one-dimensional photonic crystal coupling microcavity as claimed in claim 1, wherein the method comprises the following steps: in the step S8, the Piranha solution is used for cleaning for 10-15 min, and the HF solution is used for cleaning for 15-20S.
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Publication number Priority date Publication date Assignee Title
CN101339900A (en) * 2007-07-02 2009-01-07 旺宏电子股份有限公司 Method for surface modification of semiconductor layer and method of manufacturing semiconductor device
US9359513B1 (en) * 2010-05-07 2016-06-07 Thin Film Electronics Asa Dopant inks, methods of making dopant inks, and methods of using dopant inks
CN103645158A (en) * 2013-12-05 2014-03-19 中国电子科技集团公司第三十八研究所 Three-ring-shaped athermalized biosensor
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