CN111584707B - Double-layer adhesive stripping method for nanowire structure of SNSPD (single-wire quantum device) - Google Patents

Double-layer adhesive stripping method for nanowire structure of SNSPD (single-wire quantum device) Download PDF

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CN111584707B
CN111584707B CN202010277519.XA CN202010277519A CN111584707B CN 111584707 B CN111584707 B CN 111584707B CN 202010277519 A CN202010277519 A CN 202010277519A CN 111584707 B CN111584707 B CN 111584707B
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double
glue
layer glue
electron beam
drying
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CN111584707A (en
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汤演
刘晓宇
李�浩
尤立星
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Shanghai Institute of Microsystem and Information Technology of CAS
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    • HELECTRICITY
    • H10SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10NELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N60/00Superconducting devices
    • H10N60/01Manufacture or treatment
    • H10N60/0156Manufacture or treatment of devices comprising Nb or an alloy of Nb with one or more of the elements of group 4, e.g. Ti, Zr, Hf
    • 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
    • HELECTRICITY
    • H10SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10NELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N60/00Superconducting devices
    • H10N60/01Manufacture or treatment
    • H10N60/0241Manufacture or treatment of devices comprising nitrides or carbonitrides

Abstract

The invention relates to a double-layer glue stripping method for a nanowire structure of an SNSPD (single crystal silicon device) device, which adopts ZEP-520A electron beam resist as bottom glue of the double-layer glue and AR-P6200 electron beam resist as top glue of the double-layer glue. The two resists adopted by the invention can be developed in o-xylene, and the photoresist removing process can be simultaneously carried out in the same step, so that the process is simpler, and the sol stripping of the zigzag nanowire structure is realized by matching with various solvents; meanwhile, the undercut structure is realized by utilizing the difference of the central doses of the two resists, and the method has the advantages of simple process, good repeatability and the like.

Description

Double-layer adhesive stripping method for nanowire structure of SNSPD (single-wire quantum device)
Technical Field
The invention belongs to the field of integrated circuit engineering, and particularly relates to a double-layer adhesive stripping method for a nanowire structure of an SNSPD device.
Background
Since the first experimental report, SNSPD has been widely used in the fields of quantum communication, lidar, satellite laser ranging, and quantum random number generation, as a high-performance SPD having the advantages of high detection efficiency, low dark count, and low time jitter. The advent of single photon detectors has revolutionized the many areas of research associated with weak signal detection. The mid-infrared detection technology has extremely important application in the wide fields of basic science, medicine, daily life, military and the like. Because the structure of the current high-performance SNSPD is more and more complex, the preparation difficulty of the nanowire structure is improved due to the coupling modes such as waveguide coupling and the like, and the nanowire structure transferred by an etching mode presents greater limitation. And since the dimension of the nano-wire is usually in the order of hundreds of nanometers, the research of new process also becomes the current hot field.
CN101430503A discloses a method for removing double-layer glue for electron beam lithography stripping, which adopts LOR type resist as bottom glue of the double-layer glue and ZEP520 type electron beam resist as top glue. The problem of stripping a high-aspect-ratio structure is mainly solved, but the problem of process failure can be caused by colloid collapse under the condition that the structure scale is small because the ZEP-520 electron beam resist is sensitive to exposure dose as top glue. If the conductive silicon oxide is directly applied to the SNSPD device, because the LOR corrosion inhibitor is insensitive to electron beams, if LOR glue is used for stripping nanowires of about one hundred nanometers, an LOR corrosive agent is additionally used for corroding the LOR glue, an internally tangent structure cannot be directly formed through development, the process is complex, and the preparation efficiency of the SNSPD device is greatly influenced. Even if the exposure time is sacrificed, the prepared lines still have the condition of collapse and adhesion after compensation. Therefore, it is necessary to develop a new method for double-layer glue stripping of the nanowire structure of the SNSPD device.
Disclosure of Invention
The invention aims to solve the technical problem of providing a double-layer adhesive stripping method for a nanowire structure of an SNSPD device, which solves the problems of complex process, low yield, uncontrollable etching rate and the like in the prior art of carrying out double-layer adhesive stripping by using an LOR adhesive or etching and processing NbN nanowires by using RIE equipment.
The invention provides a double-layer adhesive stripping method for a nanowire structure of an SNSPD (single-semiconductor field-effect transistor) device, which comprises the following steps:
(1) Cleaning and drying the substrate, spin-coating a ZEP-520A electron beam resist on the substrate to serve as a bottom layer glue of the double-layer glue, and drying; then, spin-coating AR-P6200 type electron beam resist on the bottom glue to serve as the top glue of the double-layer glue, and drying;
(2) Exposing the nanowire structure of the SNSPD device by using an electron beam, and exposing the double-layer adhesive; developing, fixing and blow-drying the exposed double-layer glue by utilizing o-xylene at the same time to obtain an undercut structure photoetching pattern;
(3) Then growing a superconducting material on the obtained undercut structure photoetching pattern; and finally, simultaneously removing the top layer glue and the bottom layer glue by using various solvents to complete a stripping process to obtain the required zigzag nanowire pattern.
The spin coating speed in the step (1) is 4000rpm.
In the step (1), the temperature is 180 ℃ and the time is 5min when the bottom layer adhesive is dried; the temperature is 150 ℃ and the time is 1min when the top layer glue is dried.
The developing time in the step (2) is 49 seconds; the fixing time is 90 seconds, and isopropanol fixing solution is adopted for fixing; the blow-drying is carried out by using high-purity nitrogen.
The superconducting material in the step (3) is one or more of NbN, nb and NbTiN.
The growing method in the step (3) is magnetron sputtering and electron beam evaporation.
The step (3) of simultaneously removing the top layer glue and the bottom layer glue by using a plurality of solvents specifically comprises the following steps: firstly heating N-methyl pyrrolidone for 30 minutes at 90 ℃, then soaking the glass by clean new N-methyl pyrrolidone for 2 hours, and finally carrying out deionized water ultrasound for 5 minutes, acetone ultrasound for 5 minutes and isopropanol ultrasound for 5 minutes.
AR-P6200 (ALLRESIST. Corp.) E-Beam resist center dose 350 uC/cm used in the present invention 2 Sensitivity is higher than that of PMMA series electron beam resist, and the central dose difference with ZEP-520A electron beam resist is 100 mu C/cm 2 Left and right. Both AR-P6200 and ZEP-520A E-beam resists were verified to be developed in ortho-xylene and resist stripping was similar, so top and bottom resists used in E-beam bilayer resist were ideal. Since the AR-P6200 center dose is higher than the ZEP-520A, the primer ZEP-520A will be overexposed due to the smaller center dose. The invention adopts AR-P6200 as the top layer glue and ZEP-520A as the bottom layer glue, thereby having higher innovative significance and practical value.
Advantageous effects
The two resists adopted by the invention can be developed in o-xylene, and the photoresist removing process can be simultaneously carried out in the same step, so that the process is simpler, and the sol stripping of the zigzag nanowire structure is realized by matching with various solvents; since AR-P6200 is a highly sensitive electron beam resist, the center dose is 350 μ C/cm 2 800 μ C/cm of PMMA series electron beam resist 2 Compared with the prior art, the method has the advantages that the electron beam exposure time can be greatly shortened; compared with the double-layer glue process with the LOR as the bottom glue, the double-layer glue is only required to be developed once and removed once, so that the efficiency and the yield are higher; meanwhile, the undercut structure is realized by utilizing the difference of the central doses of the two resists, the difficulty of the stripping process is reduced, the stripping yield is improved, and the method has the advantages of simple process, good repeatability and the like.
Drawings
FIG. 1 is a process flow diagram of the present invention;
fig. 2 is an SEM image of the NbN superconducting nanowire structure prepared in example 1.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example 1
Step 1, cleaning a silicon substrate according to a microelectronic standard cleaning process, and drying;
step 2, spin-coating a layer of ZEP-520A electron beam resist with the thickness of 80nm on a silicon substrate at the rotating speed of 4000rpm as bottom glue of double-layer glue, and drying the substrate at 180 ℃ for 5 minutes by a baking table;
step 3, spin-coating AR-P6200 electron beam resist with the thickness of 80nm on the ZEP-520A layer at the rotating speed of 4000rpm as top layer glue of the double-layer glue, and drying the double-layer glue at the baking table for 1 minute at the temperature of 150 ℃;
step 4, electron beam exposure, wherein the double-layer glue is exposed with the dose of 350 mu C/cm 2 Obtaining a zigzag nanowire pattern with the line width of 120nm and the period of 200nm, wherein the bottom layer ZEP-520A electron beam resist is overexposed;
step 5, developing the sample by adopting o-xylene for 49 seconds and fixing the sample by using isopropanol for 90 seconds to simultaneously complete the development of the two electron beam resists, and drying the two electron beam resists by using high-purity nitrogen to obtain a graph with an internally tangent structure;
step 6, magnetron sputtering a superconducting material layer, namely NbN with the thickness of 8 nm;
and 7, firstly heating the NbN superconducting nanowire structure pattern for 30 minutes at 90 ℃ by adopting N-methylpyrrolidone (NMP), then soaking the NbN superconducting nanowire structure pattern for 2 hours by adopting clean new NMP, and finally carrying out ultrasonic treatment on deionized water for 5 minutes, acetone ultrasonic treatment for 5 minutes and isopropanol ultrasonic treatment for 5 minutes to simultaneously complete the degumming of the top layer glue and the bottom layer glue and complete the stripping process to obtain the NbN superconducting nanowire structure pattern.
As can be seen from FIG. 2, the NbN superconducting nanowire with the thickness of 8nm and the line width of 120nm prepared by stripping according to the method has a clear structure and clear line edges. The stripping and photoresist removing effect is good, and no obvious residual photoresist phenomenon exists. The prepared structure can be applied to subsequent processes.
Example 2
Step 1, cleaning a 1550nm high-reflectivity substrate according to a microelectronic standard cleaning process, and drying;
step 2, spin-coating a layer of ZEP-520A electron beam resist with the thickness of 80nm on a high-contrast substrate at the rotating speed of 4000rpm as bottom glue of double-layer glue, and drying the substrate at 180 ℃ for 5 minutes by a baking table;
step 3, spin-coating AR-P6200 electron beam resist with the thickness of 80nm on the ZEP-520A layer at the rotating speed of 4000rpm as top layer glue of the double-layer glue, and drying the double-layer glue at the baking table for 1 minute at the temperature of 150 ℃;
step 4, electron beam exposure, wherein the double-layer glue is exposed, and the dosage adopts 400 mu C/cm in consideration of the multi-layer structure of the 1550nm high-reflection substrate 2 Obtaining a zigzag nanowire pattern with the line width of 80nm and the period of 160nm, and overexposing the bottom layer ZEP-520A electron beam resist;
step 5, developing the sample by adopting o-xylene for 49 seconds and fixing the sample by using isopropanol for 90 seconds to simultaneously complete the development of the two electron beam resists, and drying the two electron beam resists by using high-purity nitrogen to obtain a graph with an internally tangent structure;
step 6, magnetron sputtering a superconducting material layer, namely NbN with the thickness of 6.5 nm;
and 7, firstly heating the substrate for 30 minutes at 90 ℃ by adopting N-methylpyrrolidone (NMP), then soaking the substrate for 2 hours by adopting clean new NMP, finally performing ultrasonic treatment on deionized water for 5 minutes, performing ultrasonic treatment on acetone for 5 minutes and performing ultrasonic treatment on isopropanol for 5 minutes, simultaneously removing the top layer glue and the bottom layer glue, and completing a stripping process to obtain the NbN superconducting nanowire structural graph.
In conclusion, the invention effectively solves the problems that the developing photoresist removing process is complex, the materials are easy to adhere, the photoresist is difficult to remove, the etching rate of the nanowire prepared by the etching process is difficult to control and the like in the conventional electron beam double-layer photoresist stripping technology.

Claims (7)

1. A double-layer adhesive stripping method for a nanowire structure of a SNSPD device comprises the following steps:
(1) Cleaning and drying the substrate, spin-coating a ZEP-520A electron beam resist on the substrate to serve as a bottom layer glue of the double-layer glue, and drying; then, spin-coating AR-P6200 type electron beam resist on the bottom glue to serve as the top glue of the double-layer glue, and drying;
(2) Exposing the nanowire structure of the SNSPD device by an electron beam, and exposing the double-layer adhesive; developing, fixing and blow-drying the exposed double-layer glue by utilizing o-xylene at the same time to obtain an undercut structure photoetching pattern;
(3) Then growing a superconducting material on the obtained undercut structure photoetching pattern; and finally, simultaneously removing the top layer glue and the bottom layer glue by using various solvents to complete a stripping process, thereby obtaining the required zigzag nanowire pattern.
2. The method of claim 1, wherein: the spin coating speed in the step (1) is 4000rpm.
3. The method of claim 1, wherein: in the step (1), the temperature is 180 ℃ and the time is 5min when the bottom layer adhesive is dried; the temperature for drying the top layer glue is 150 ℃ and the time is 1min.
4. The method of claim 1, wherein: the developing time in the step (2) is 49 seconds; the fixing time is 90 seconds, and isopropanol fixing solution is adopted for fixing; the blow-drying is carried out by using high-purity nitrogen.
5. The method of claim 1, wherein: the superconducting material in the step (3) is one or more of NbN, nb and NbTiN.
6. The method of claim 1, wherein: the growing method in the step (3) comprises magnetron sputtering and electron beam evaporation.
7. The method of claim 1, wherein: the step (3) of simultaneously removing the top layer glue and the bottom layer glue by using a plurality of solvents specifically comprises the following steps: firstly heating N-methyl pyrrolidone for 30 minutes at 90 ℃, then soaking the glass by clean new N-methyl pyrrolidone for 2 hours, and finally carrying out deionized water ultrasound for 5 minutes, acetone ultrasound for 5 minutes and isopropanol ultrasound for 5 minutes.
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