LabAdviser/Technology Research/Fabrication of Hyperbolic Metamaterials using Atomic Layer Deposition/TIO ALU Gratings Procces flow: Difference between revisions

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'''Feedback to this page''': '''[mailto:labadviser@nanolab.dtu.dk?Subject=Feed%20back%20from%20page%20http://labadviser.nanolab.dtu.dk/index.php/LabAdviser/Technology_Research/Fabrication_of_Hyperbolic_Metamaterials_using_Atomic_Layer_Deposition/TIO_ALU_Gratings_Procces_flow click here]'''
<i>This page is written by <b>Evgeniy Shkondin @DTU Nanolab</b> if nothing else is stated. <br>
All images and photos on this page belongs to <b>DTU Nanolab</b> and <b>DTU Electro</b> (previous DTU Fotonik).<br>
The fabrication and characterization described below were conducted in <b>2013-2016 by Evgeniy Shkondin, DTU Nanolab</b>.<br></i>
====Procces flow description====
====Procces flow description====


The substrates for the samples were fabricated by depositing 1 μm of Si<sub>3</sub>N<sub>4</sub> (the resonator layer) on 100 mm silicon < 100 > wafers using low-pressure chemical vapor deposition. The process was carried out at 780C with ammonia (NH<sub>3</sub>) and dichlorosilane (SiH<sub>2</sub>Cl<sub>2</sub>) as reactive gases. Thickness and refractive index of the deposited silicon nitride was measured and confirmed using spectroscopic ellipsometry. The deposited Si<sub>3</sub>N<sub>4</sub> film was carefully analyzed for existence of cracks, particles and other defects using dark field optical microscopy. The best-quality wafer with Si<sub>3</sub>N<sub>4</sub> was selected and cleaved in pieces, which were used as substrates for the deposition of Al<sub>2</sub>O<sub>3</sub>/TiO<sub>2</sub> multilayers. Before inserting each substrate into the ALD reactor, it was placed on a Si carrier wafer. Therefore the Al<sub>2</sub>O<sub>3</sub>/TiO<sub>2</sub> multilayers were grown not only on the Si<sub>3</sub>N<sub>4</sub> layer but also on the dummy carrier wafer. After the ALD process was completed, the dummy was cleaved and its cross-section was characterized using scanning electron microscopy (SEM). The SEM images reveal high-quality homogeneous, conformal coatings, as seen in the examples in Figs 1. Such a method of deposited multilayers characterization turned out to be more feasible than the direct SEM characterization of multilayers on Si<sub>3</sub>N<sub>4</sub>, since the latter suffers from issues related to charge accumulation on the silicon nitride.
All samples were prepared and characterized in a class 100 cleanroom. Si (100) wafers of 150 mm were used as a substrate. The main steps in the gratings manufacturing are shown in a figure below. First, the silicon trenches were realized by deep reactive ion etching (DRIE). Then, the trenches were ALD coated. After the selective removal of the top parts, the silicon core between ALD coatings was etched away during the last step. The final structure represents the highly anisotropic vertical grating. Each fabrication step was carefully inspected using cross-sectional scanning electron microscopy (SEM) imaging.
 


<gallery caption="" widths="1000px" heights="600px" perrow="1">
image:nanogratings_sheme.jpg| Scheme of fabrication flow. High aspect ratio Al<sub>2</sub>O<sub>3</sub> and TiO<sub>2</sub> nanogratings.
</gallery>


<gallery caption="" widths="1000px" heights="600px" perrow="1">
<gallery caption="" widths="1000px" heights="600px" perrow="1">
image:TIO_ALU_Gratings_SEM.jpg| High aspect ratio Al<sub>2</sub>O<sub>3</sub> and TiO<sub>2</sub> nanogratings.
image:TIO_ALU_Gratings_SEM.jpg| High aspect ratio Al<sub>2</sub>O<sub>3</sub> and TiO<sub>2</sub> nanogratings. SEM cross-sectional inspection.
</gallery>
</gallery>


== Process flow ==
== Process flow ==
Hej Evgeniy <br>
Description of steps for fabrication of TiO<sub>2</sub> and AL<sub>2</sub>O<sub>3</sub> nanogratings.
Jeg har lagt dette eksemple på et process flow ind. Alt tekst og billeder skal selvfølgelig erstattes af relevante process steps for denne artikel.
 
Mvh. Berit


{| border="1" cellspacing="1" cellpadding="3" style="text-align: left; width: 925px; height: 220px;"
{| border="1" cellspacing="1" cellpadding="3" style="text-align: left; width: 925px; height: 220px;"
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|-
|-
!2.1
!1.1
|Plasma surface treatment
|Plasma surface treatment
|To ensure clean surface, the 100 mm Si wafer is treated by O<sub>2</sub>/N<sub>2</sub> plasma. (Optional step)
|To ensure clean surface, the 100 mm Si wafer is treated by O<sub>2</sub>/N<sub>2</sub> plasma. (Optional step)
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|-
|-
|- style="background:#BCD4E6; color:black"
|- style="background:#BCD4E6; color:black"
!2.2
!1.2
|DUV Resist patterning
|DUV Resist patterning
|DUV
|DUV
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|-
|-
!2.3
!1.3
|Deep reactive ion etching (DRIE)
|Deep reactive ion etching (DRIE)
|DRIE  
|DRIE; [[Specific_Process_Knowledge/Etch/DRIE-Pegasus/DUVetch|Recipe: PolySOI10]]
| [[Specific_Process_Knowledge/Etch/DRIE-Pegasus|DRIE Pegasus]].
| [[Specific_Process_Knowledge/Etch/DRIE-Pegasus|DRIE Pegasus]].
|[[image:00_zero (3)_nanogratings.JPG|250x350px|center|]]
|[[image:00_zero (3)_nanogratings.JPG|250x350px|center|]]
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|-
|-
|- style="background:#BCD4E6; color:black"
|- style="background:#BCD4E6; color:black"
!2.4
!1.4
|Plasma surface treatment
|Plasma surface treatment
|To ensure that remainings of DUV resist are gone, samples are treated by O<sub>2</sub>/N<sub>2</sub> plasma. (Optional step)
|To ensure that remainings of DUV resist are gone, samples are treated by O<sub>2</sub>/N<sub>2</sub> plasma. (Optional step)
|[[Specific_Process_Knowledge/Lithography/Strip#Plasma_Asher_2| Plasma Asher 2]].
|[[Specific_Process_Knowledge/Lithography/Strip#Plasma_Asher_2| Plasma Asher 2]].
|[[no image]]
|
|-
|-


|-
|-
!2.5
!1.5
|Scanning Electron Microscopy inspection  
|Scanning Electron Microscopy inspection  
|By cleaving the sample it is possible to inspect DRIE etched Si trenches in cross-sectional mode
|By cleaving the sample it is possible to inspect DRIE etched Si trenches in cross-sectional mode
|[[Specific_Process_Knowledge/Characterization/SEM_Supra_2|SEM Supra 2]]  
|
[[Specific_Process_Knowledge/Characterization/SEM_Supra_1|SEM Supra 1]]
<br clear="all" />
[[Specific_Process_Knowledge/Characterization/SEM_Supra_2|SEM Supra 2]]
<br clear="all" />
[[Specific_Process_Knowledge/Characterization/SEM_Supra_3|SEM Supra 3]]
|[[image:Si_trenches_nanogratings.jpg|250x350px|center]]
|[[image:Si_trenches_nanogratings.jpg|250x350px|center]]
|-
|-
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|-
|-
|- style="background:#BCD4E6; color:black"
|- style="background:#BCD4E6; color:black"
!2.6
!1.6
|Atomic Layer Deposition of either Al<sub>2</sub>O<sub>3</sub> or TiO<sub>2</sub>
|Atomic Layer Deposition of either Al<sub>2</sub>O<sub>3</sub> or TiO<sub>2</sub>
|Deposition carried at 150C.Thickness is 90 nm.
|Deposition carried at 150C.Thickness is 90 nm.
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|-
|-
|- style="background:#BCD4E6; color:black"
!1.7
!2.7
|Scanning Electron Microscopy inspection
|Scanning Electron Microscopy inspection
|By cleaving the sample it is possible to inspect ALD coatings deposited on Si trenches in cross-sectional mode
|By cleaving the sample it is possible to inspect ALD coatings deposited on Si trenches in cross-sectional mode
|[[Specific_Process_Knowledge/Characterization/SEM_Supra_2|SEM Supra 2]]
|
|[[image:Si_trenches_nanogratings.jpg|250x350px|center]]  
[[Specific_Process_Knowledge/Characterization/SEM_Supra_1|SEM Supra 1]]
<br clear="all" />
[[Specific_Process_Knowledge/Characterization/SEM_Supra_2|SEM Supra 2]]
<br clear="all" />
[[Specific_Process_Knowledge/Characterization/SEM_Supra_3|SEM Supra 3]]
|[[image:TiO2_coating_nanogratings.jpg|250x350px|center]]  
|-
|-


|-
|-
|- style="background:#BCD4E6; color:black"
|- style="background:#BCD4E6; color:black"
!2.8
!1.8
|Opening of deposited Al<sub>2</sub>O<sub>3</sub> or TiO<sub>2</sub> top layers.
|Opening of deposited Al<sub>2</sub>O<sub>3</sub> or TiO<sub>2</sub> top layers.
|Etching happens using ICP Metal etcher with Cl<sub>2</sub>/BCl<sub>3</sub> process gasses.
|Etching happens using ICP Metal etcher with Cl<sub>2</sub>/BCl<sub>3</sub> process gasses.
||Equipment used: [[Specific_Process_Knowledge/Etch/ICP_Metal_Etcher|Metal ICP Etcher]].  
||Equipment used: [[Specific_Process_Knowledge/Etch/ICP_Metal_Etcher|Metal ICP Etcher]].  
  |[[image:00_zero (5)_nanogratings.JPG|250x350px|center]]
  |[[image:00_zero (6)_nanogratings.JPG|250x350px|center]]
|-
 
 
|-
!1.9
|Scanning Electron Microscopy inspection
|By cleaving the sample it is possible to inspect ICP etcher results Si trenches in cross-sectional mode
|
[[Specific_Process_Knowledge/Characterization/SEM_Supra_1|SEM Supra 1]]
<br clear="all" />
[[Specific_Process_Knowledge/Characterization/SEM_Supra_2|SEM Supra 2]]
<br clear="all" />
[[Specific_Process_Knowledge/Characterization/SEM_Supra_3|SEM Supra 3]]
|[[image:TiO2_top_removal_nanogratings.jpg|250x350px|center]]
|-
 
|-
|- style="background:#BCD4E6; color:black"
!1.10
|Selective etch of Si between ALD  Al<sub>2</sub>O<sub>3</sub> or TiO<sub>2</sub> coatings.
|Si etching proceeds using ICP Metal etcher with isotropic  process based on SF<sub>f</sub> process gas.
||Equipment used: [[Specific_Process_Knowledge/Etch/ICP_Metal_Etcher|Metal ICP Etcher]].
|[[image:00_zero (7)_nanogratings.JPG|250x350px|center]]
|-
 
 
|-
!1.11
|Scanning Electron Microscopy inspection of fabricated structure.
|Proof of final result.
|
[[Specific_Process_Knowledge/Characterization/SEM_Supra_1|SEM Supra 1]]
<br clear="all" />
[[Specific_Process_Knowledge/Characterization/SEM_Supra_2|SEM Supra 2]]
<br clear="all" />
[[Specific_Process_Knowledge/Characterization/SEM_Supra_3|SEM Supra 3]]
|[[image:TiO2_grating_nanogratings.jpg|250x350px|center]]  
|-
|-


|-
|- style="background:#BCD4E6; color:black"
!1.12
|Ion beam etching. (Optional)
|Additional shape of the top part. 20 mijn etch using recipe [[Specific_Process_Knowledge/Etch/IBE⁄IBSD_Ionfab_300/IBE_Ti_etch|"Ti acceptance"]] there the stage shoud be placed to 0<sup>o</sup> degree. SEM cross section is used for inspection
|[[Specific_Process_Knowledge/Etch/IBE⁄IBSD_Ionfab_300|IBE/IBSD Ionfab 300]]
|[[image:image1004_nanogratings.jpg|250x350px|center]]
|-


|-
|-
|}
|}
<br clear="all" />
<br clear="all" />

Latest revision as of 14:43, 2 February 2023

Feedback to this page: click here

This page is written by Evgeniy Shkondin @DTU Nanolab if nothing else is stated.
All images and photos on this page belongs to DTU Nanolab and DTU Electro (previous DTU Fotonik).
The fabrication and characterization described below were conducted in 2013-2016 by Evgeniy Shkondin, DTU Nanolab.

Procces flow description

All samples were prepared and characterized in a class 100 cleanroom. Si (100) wafers of 150 mm were used as a substrate. The main steps in the gratings manufacturing are shown in a figure below. First, the silicon trenches were realized by deep reactive ion etching (DRIE). Then, the trenches were ALD coated. After the selective removal of the top parts, the silicon core between ALD coatings was etched away during the last step. The final structure represents the highly anisotropic vertical grating. Each fabrication step was carefully inspected using cross-sectional scanning electron microscopy (SEM) imaging.


Process flow

Description of steps for fabrication of TiO2 and AL2O3 nanogratings.

Step Description LabAdviser link Image showing the step
1.1 Plasma surface treatment To ensure clean surface, the 100 mm Si wafer is treated by O2/N2 plasma. (Optional step) Plasma Asher 2
00 zero (1) nanogratings.JPG
1.2 DUV Resist patterning DUV DUV Stepper Lithography.
00 zero (2) nanogratings.JPG
1.3 Deep reactive ion etching (DRIE) DRIE; Recipe: PolySOI10 DRIE Pegasus.
00 zero (3) nanogratings.JPG
1.4 Plasma surface treatment To ensure that remainings of DUV resist are gone, samples are treated by O2/N2 plasma. (Optional step) Plasma Asher 2.
1.5 Scanning Electron Microscopy inspection By cleaving the sample it is possible to inspect DRIE etched Si trenches in cross-sectional mode

SEM Supra 1
SEM Supra 2
SEM Supra 3

Si trenches nanogratings.jpg
1.6 Atomic Layer Deposition of either Al2O3 or TiO2 Deposition carried at 150C.Thickness is 90 nm. Equipment used: ALD Picosun R200. Standard recipes used: Al2O3T and TiO2T .
00 zero (4) nanogratings.JPG
1.7 Scanning Electron Microscopy inspection By cleaving the sample it is possible to inspect ALD coatings deposited on Si trenches in cross-sectional mode

SEM Supra 1
SEM Supra 2
SEM Supra 3

TiO2 coating nanogratings.jpg
1.8 Opening of deposited Al2O3 or TiO2 top layers. Etching happens using ICP Metal etcher with Cl2/BCl3 process gasses. Equipment used: Metal ICP Etcher.
00 zero (6) nanogratings.JPG
1.9 Scanning Electron Microscopy inspection By cleaving the sample it is possible to inspect ICP etcher results Si trenches in cross-sectional mode

SEM Supra 1
SEM Supra 2
SEM Supra 3

TiO2 top removal nanogratings.jpg
1.10 Selective etch of Si between ALD Al2O3 or TiO2 coatings. Si etching proceeds using ICP Metal etcher with isotropic process based on SFf process gas. Equipment used: Metal ICP Etcher.
00 zero (7) nanogratings.JPG
1.11 Scanning Electron Microscopy inspection of fabricated structure. Proof of final result.

SEM Supra 1
SEM Supra 2
SEM Supra 3

TiO2 grating nanogratings.jpg
1.12 Ion beam etching. (Optional) Additional shape of the top part. 20 mijn etch using recipe "Ti acceptance" there the stage shoud be placed to 0o degree. SEM cross section is used for inspection IBE/IBSD Ionfab 300
Image1004 nanogratings.jpg