CN117865218A - Dry deep etching process for thin film lithium niobate - Google Patents
Dry deep etching process for thin film lithium niobate Download PDFInfo
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- CN117865218A CN117865218A CN202311751382.7A CN202311751382A CN117865218A CN 117865218 A CN117865218 A CN 117865218A CN 202311751382 A CN202311751382 A CN 202311751382A CN 117865218 A CN117865218 A CN 117865218A
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- lithium niobate
- thin film
- film lithium
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- GQYHUHYESMUTHG-UHFFFAOYSA-N lithium niobate Chemical compound [Li+].[O-][Nb](=O)=O GQYHUHYESMUTHG-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 239000010409 thin film Substances 0.000 title claims abstract description 59
- 238000005530 etching Methods 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 43
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 35
- 238000010894 electron beam technology Methods 0.000 claims description 33
- 229910052804 chromium Inorganic materials 0.000 claims description 32
- 239000011651 chromium Substances 0.000 claims description 32
- 238000001312 dry etching Methods 0.000 claims description 25
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 24
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 22
- 239000010408 film Substances 0.000 claims description 22
- XPDWGBQVDMORPB-UHFFFAOYSA-N Fluoroform Chemical compound FC(F)F XPDWGBQVDMORPB-UHFFFAOYSA-N 0.000 claims description 20
- 239000003292 glue Substances 0.000 claims description 19
- 239000007789 gas Substances 0.000 claims description 16
- 235000012239 silicon dioxide Nutrition 0.000 claims description 12
- 239000000377 silicon dioxide Substances 0.000 claims description 12
- 229910052786 argon Inorganic materials 0.000 claims description 11
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000004528 spin coating Methods 0.000 claims description 10
- 229910052710 silicon Inorganic materials 0.000 claims description 9
- 239000010703 silicon Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000009616 inductively coupled plasma Methods 0.000 claims description 7
- 238000000151 deposition Methods 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 238000005566 electron beam evaporation Methods 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 230000008021 deposition Effects 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 2
- 230000003287 optical effect Effects 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- 230000001276 controlling effect Effects 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 13
- 235000012431 wafers Nutrition 0.000 description 7
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000001000 micrograph Methods 0.000 description 4
- 238000004506 ultrasonic cleaning Methods 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 210000001520 comb Anatomy 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 238000011010 flushing procedure Methods 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000004891 communication Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000009022 nonlinear effect Effects 0.000 description 1
- 238000001020 plasma etching Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 125000002023 trifluoromethyl group Chemical group FC(F)(F)* 0.000 description 1
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- Drying Of Semiconductors (AREA)
Abstract
The invention relates to the technical field of optical materials, in particular to a dry deep etching process of thin film lithium niobate. According to the invention, the etching speed and effect of lithium niobate can be regulated and controlled by controlling the air pressure, proportion and etching time of etching gas. The thin film lithium niobate device with the etching depth exceeding 500nm, the side wall roughness being less than 10nm and the side wall inclination exceeding 75 degrees can be obtained.
Description
Technical Field
The invention relates to the technical field of optical materials, in particular to a dry deep etching process of thin film lithium niobate.
Background
Lithium niobate is a good optical material and has wide application prospect in the fields of optical communication, quantum optics and the like. The high-speed electro-optic modulator has a large electro-optic coefficient and is widely applied to high-speed electro-optic modulators; the method has a large second-order nonlinear coefficient and is used for sum frequency, difference frequency effect and quantum light source; the method has three-order nonlinear coefficients at the same time, and can be used for generating Kerr frequency combs.
Research on lithium niobate has begun since the sixties of the twentieth century. Conventional lithium niobate devices are based on lithium niobate bulk materials that utilize ion exchange to achieve low index-contrast waveguides. The low refractive index difference waveguide has weak local effect on light, large space volume and limited nonlinear effect, so that the traditional lithium niobate device has larger volume, is difficult to integrate and is greatly limited in application.
At the beginning of the twenty-first century, researchers achieved high quality thin film lithium niobate wafers through ion dicing and wafer bonding techniques. More important, the breakthrough of the dry etching process of the thin film lithium niobate provides a new technical route for realizing the thin film lithium niobate waveguide with ultralow loss and high refractive index difference. On this basis, researchers have developed a variety of functional devices based on thin film lithium niobate, such as: integrated broadband high-speed electro-optic modulators, on-chip compression generation, on-chip Kerr frequency combs, and the like.
In order to realize high-quality optical structures such as thin film lithium niobate waveguides, micro-rings and the like, researchers have proposed various dry etching schemes. One common approach is to use an argon plasma for etching, with masks typically utilizing electron beam resist (e.g., HSQ resist, ZEP resist, etc.), hard masks (e.g., silicon dioxide), and metal masks (e.g., chrome masks), etc. Etching with an argon plasma can effectively improve the sidewall roughness of the etch, but this approach has some drawbacks, such as difficulty in achieving deep etching with high sidewall sharpness for thin film lithium niobate.
Disclosure of Invention
The invention provides a dry-method deep etching process of thin-film lithium niobate, which can realize the etching results of deep etching (with depth more than 500 nm) and high sidewall verticality (more than 75 ℃).
The invention provides a dry etching method of film lithium niobate, comprising the following steps: argon and trifluoromethane were used as etching gases.
According to the dry etching method of the film lithium niobate, the volume ratio of argon to trifluoromethane is 0.8-1.2:0.8-1.2; preferably 0.9-1.1:0.9-1.1; further preferably 1:1.
According to the thin film lithium niobate dry etching method, the etching time is 10 to 20 minutes, preferably 12 to 17 minutes, and more preferably 15 minutes.
According to the dry etching method of the film lithium niobate, the gas flow rate is 18-27sccm; preferably 20-25sccm; further preferably 20sccm.
The radio frequency power is 50-300W; preferably 180-220W; further preferably 190-210; more preferably 200W.
According to the dry etching method of the film lithium niobate, a layer of electron beam glue is spin-coated on the surface of the film lithium niobate sample, and the pattern is transferred to the electron beam glue through electron beam exposure.
According to the thin film lithium niobate dry etching method, metal chromium is deposited on the surface of a wafer according to the thin film lithium niobate dry etching method, and the pattern is transferred to a chromium mask through a lift-off process.
And etching by adopting an inductive coupling plasma etching method according to the dry etching method of the film lithium niobate.
According to the thin film lithium niobate dry etching method, a thin film lithium niobate sample comprises a thin film lithium niobate layer, a silicon dioxide layer and a silicon layer.
The dry etching method of the thin film lithium niobate comprises the following steps:
cleaning a film lithium niobate sample to be processed;
spin-coating electron beam glue on the surface of the sample, transferring a pattern onto the electron beam glue through electron beam exposure, and developing;
depositing a chromium film on the surface of the sample by using electron beam evaporation deposition equipment;
washing off the residual electron beam glue to obtain a chromium mask;
placing the sample in ICP equipment, and etching the sample;
immersing the sample in a mixed solution of hydrogen peroxide, ammonia water and water;
and immersing the sample in a chromium removing agent to clean the chromium mask remained on the surface, thus obtaining the thin film lithium niobate device.
Preferably, the specific flow based on the physicochemical dry etching in the invention is as follows:
1) And cleaning a thin film lithium niobate sample to be processed, wherein the sample comprises a thin film lithium niobate layer, a silicon dioxide layer and a silicon layer, the thickness of the thin film lithium niobate layer is 600nm, the thickness of the silicon dioxide layer is 4000nm, and the thickness of the silicon layer is 0.5mm.
2) Spin-coating electron beam glue on the surface of the sample, transferring the pattern onto the electron beam glue through electron beam exposure, and developing.
3) And (3) depositing a chromium film on the surface of the sample by using an electron beam evaporation deposition device, wherein the thickness of the chromium film is 200nm.
4) And (5) cleaning the residual electron beam glue to obtain the chromium mask.
5) The sample was placed in an ICP apparatus and etched. The etching gas is a mixed gas of argon and trifluoromethane, and the gas ratio is 1:1, the gas flow rate is 20-25sccm, the radio frequency power is 50-300W, and the etching speed of the film lithium niobate is 10-50nm/min.
6) The above sample was immersed in a mixed solution of hydrogen peroxide, ammonia water and water for one hour.
7) And immersing the sample in a chromium removing agent to clean the chromium mask remained on the surface, thus obtaining the thin film lithium niobate device.
The invention also provides a thin film lithium niobate device which is prepared by the thin film lithium niobate dry etching method.
The invention provides a dry etching process of a thin film lithium niobate based on physicochemical etching, which can realize the etching results of deep etching (depth is more than 500 nm) and high sidewall verticality (more than 75 degrees).
Drawings
In order to more clearly illustrate the technical solutions of the present invention or of the prior art, the following description will make a brief introduction to the drawings used as required in the description of the embodiments or of the prior art.
Fig. 1 is a flow chart of a dry deep etching process of the thin film lithium niobate provided by the invention.
Fig. 2 is an electron microscope image of a lithium niobate waveguide having an etching depth of 510nm provided in example 1 of the present invention.
Fig. 3 is an electron microscope image of a lithium niobate waveguide having an etching depth of 310nm provided in example 2 of the present invention.
Fig. 4 is an electron microscope image of a lithium niobate waveguide having an etching depth of 310nm provided in example 2 of the present invention.
Fig. 5 is an electron microscope image of a lithium niobate waveguide having an etching depth of 310nm provided in example 2 of the present invention.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings, and it is apparent that the described embodiments are some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The existing masks for etching the film lithium niobate comprise three main types of electron beam glue, silicon dioxide and metal masks, and chromium masks have outstanding advantages compared with other two types. The electron beam glue has low selection ratio and high consumption speed in etching, and is unfavorable for realizing deep etching. The silicon dioxide mask has low selectivity, and can react with the trifluoromethyl, so that the physicochemical etching can not be performed. The chromium mask has large selection ratio, is easy to realize deep etching, does not react with the trifluoromethane, and can use the mixed gas of argon and the trifluoromethane to carry out physicochemical dry etching, thereby realizing the deep etching with high sidewall verticality.
The invention adopts electron beam Exposure (EBL) and inductively coupled plasma etching (ICP) methods for etching, and the process flow is shown in figure 1. The thin film lithium niobate wafer is formed by a thin film lithium niobate layer from top to bottomThe silicon dioxide layer and the silicon substrate. First, spin coating a layer of electron beam glue on the surface of a wafer, and transferring a pattern onto the electron beam glue through electron beam exposure. After development, a layer of metallic chromium is deposited on the wafer surface and the pattern is transferred to a chromium mask by lift-off process. Thereafter, the wafer is etched using ICP, and the etching gas is selected from argon (Ar) and trifluoromethane (CHF) 3 ) Is a mixed gas of (a) and (b).
Example 1
The embodiment provides a preparation method of a thin film lithium niobate device, which comprises the following steps:
1) And obtaining a film lithium niobate sample to be processed. Comprises a thin film lithium niobate layer, a silicon dioxide layer and a silicon layer, wherein the thickness of the thin film lithium niobate layer is 600nm, the thickness of the silicon dioxide layer is 4000nm, and the thickness of the silicon layer is 0.5mm.
2) The sample was washed and dried. And (3) placing the sample into an acetone solution for ultrasonic cleaning for 5 minutes, then placing into an ethanol solution for ultrasonic cleaning for 5 minutes, taking out, flushing with deionized water, and drying by using an air gun.
3) Spin-coating electron beam glue. Placing the sample in the middle of a vacuum adsorption disc of a spin coater, setting the rotating speed to 1000r/min, dripping ZEP electron beam glue in the center of the sample, carrying out spin coating, and taking down the sample after the spin coating is finished.
4) And E, electron beam exposure. Mask patterns were prepared on lithium niobate thin film samples using an electron beam exposure machine.
5) And (5) developing. The sample is soaked in a developing solution for development, then rinsed with deionized water, and the surface moisture is dried.
6) And (5) evaporating a chromium film. A 200nm thick chromium film was deposited on the sample surface using an electron beam evaporation coating apparatus.
7) And (5) lifting off. The sample was immersed in a butanone solution for 10 minutes and the pattern was transferred to the chrome mask by lift-off process.
8) And etching the film lithium niobate. Argon and trifluoromethane were used as etching gases, ratio 1:1, the gas flow rate is set to 20sccm, the radio frequency power is set to 200W, and etching is performed for 15 minutes.
9) And (5) chemical polishing. The sample was immersed in a mixed solution of hydrogen peroxide, ammonia and water for one hour.
10 A) removing the chromium mask. And immersing the sample in a chromium removing agent to clean the chromium mask remained on the surface, thus obtaining the thin film lithium niobate device.
The finished lithium niobate thin film waveguide is shown in fig. 2, and has an etching depth of 510nm, a waveguide width (top) of 700nm, and a sidewall inclination of 75 °.
Example 2
The embodiment provides a preparation method of a thin film lithium niobate device, which comprises the following steps:
1) And obtaining a film lithium niobate sample to be processed. Comprises a thin film lithium niobate layer, a silicon dioxide layer and a silicon layer, wherein the thickness of the thin film lithium niobate layer is 500nm, the thickness of the silicon dioxide layer is 4000nm, and the thickness of the silicon layer is 0.5mm
2) The sample was washed and dried. And (3) placing the sample into an acetone solution for ultrasonic cleaning for 5 minutes, then placing into an ethanol solution for ultrasonic cleaning for 5 minutes, taking out, flushing with deionized water, and drying by using an air gun.
3) Spin-coating electron beam glue. Placing the sample in the middle of a vacuum adsorption disc of a spin coater, setting the rotating speed to 1000r/min, dripping ZEP electron beam glue in the center of the sample, carrying out spin coating, and taking down the sample after the spin coating is finished.
4) And E, electron beam exposure. Mask patterns were prepared on lithium niobate thin film samples using an electron beam exposure machine.
5) And (5) developing. The sample is soaked in a developing solution for development, then rinsed with deionized water, and the surface moisture is dried.
6) And (5) evaporating a chromium film. A 200nm thick chromium film was deposited on the sample surface using an electron beam evaporation coating apparatus.
7) And (5) lifting off. The sample was immersed in a butanone solution for 10 minutes and the pattern was transferred to the chrome mask by lift-off process.
8) And etching the film lithium niobate. Argon and trifluoromethane were used as etching gases, ratio 1:1, the gas flow rate is set to 20sccm, the radio frequency power is set to 200W, and etching is performed for 10 minutes.
9) And (5) chemical polishing. The sample was immersed in a mixed solution of hydrogen peroxide, ammonia and water for one hour.
10 A) removing the chromium mask. And immersing the sample in a chromium removing agent to clean the chromium mask remained on the surface, thus obtaining the thin film lithium niobate device.
The finished lithium niobate thin film waveguide is shown in fig. 3-5, and has an etching depth of 310nm, a waveguide width (top) of 720nm, and a sidewall inclination of 75.6 °.
The etching speed and effect of lithium niobate can be regulated and controlled by controlling the air pressure, proportion and etching time of etching gas. At present, a thin film lithium niobate device with etching depth exceeding 500nm, sidewall roughness less than 10nm and sidewall inclination exceeding 75 degrees can be obtained. Fig. 2, 3, 4, and 5 are electron microscope pictures of the thin film lithium niobate waveguide obtained by the above-described process flow.
The invention provides a chromium mask-based thin film lithium niobate physical and chemical dry etching scheme, which can realize a thin film lithium niobate device with deep etching, high sidewall verticality and low roughness.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. The dry etching method of the thin film lithium niobate is characterized by comprising the following steps of: argon and trifluoromethane were used as etching gases.
2. The method for dry etching of thin film lithium niobate according to claim 1, wherein the volume ratio of argon to trifluoromethane is 0.8-1.2:0.8-1.2; preferably 0.9-1.1:0.9-1.1; further preferably 1:1.
3. Dry etching method of thin film lithium niobate according to claim 1 or 2, characterized in that the etching time is 10-20 minutes, preferably 12-17 minutes, further preferably 15 minutes.
4. A method of dry etching thin film lithium niobate according to any of claims 1 to 3, wherein the gas flow rate is 18 to 27sccm; preferably 20-25sccm; further preferably 20sccm;
the radio frequency power is 50-300W; preferably 180-220W; further preferably 190-210; more preferably 200W.
5. The method according to any one of claims 1 to 4, wherein an electron beam resist is spin-coated on the surface of the thin film lithium niobate sample, and the pattern is transferred onto the electron beam resist by electron beam exposure.
6. The method of dry etching thin film lithium niobate according to any of claims 1 to 5, wherein metallic chromium is deposited on the wafer surface and the pattern is transferred to the chromium mask by lift-off process.
7. The method according to any one of claims 1 to 6, wherein the etching is performed by an inductively coupled plasma etching method.
8. The method of dry etching thin film lithium niobate according to any of claims 1 to 7, wherein the thin film lithium niobate sample comprises a thin film lithium niobate layer, a silicon dioxide layer, and a silicon layer.
9. The method for dry etching of thin film lithium niobate according to claim 1, comprising the steps of:
cleaning a film lithium niobate sample to be processed;
spin-coating electron beam glue on the surface of the sample, transferring a pattern onto the electron beam glue through electron beam exposure, and developing;
depositing a chromium film on the surface of the sample by using electron beam evaporation deposition equipment;
washing off the residual electron beam glue to obtain a chromium mask;
placing the sample in ICP equipment, and etching the sample;
immersing the sample in a mixed solution of hydrogen peroxide, ammonia water and water;
and immersing the sample in a chromium removing agent to clean the chromium mask remained on the surface, thus obtaining the thin film lithium niobate device.
10. A thin film lithium niobate device, characterized in that it is prepared by the thin film lithium niobate dry etching method according to any one of claims 1 to 9.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311751382.7A CN117865218A (en) | 2023-12-19 | 2023-12-19 | Dry deep etching process for thin film lithium niobate |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311751382.7A CN117865218A (en) | 2023-12-19 | 2023-12-19 | Dry deep etching process for thin film lithium niobate |
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