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====Procces flow description====
'''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/AZO_gratings 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></i>
 
 
=Fabrication of Hyperbolic Metamaterials by ALD: AZO Gratings=
 
The fabrication and characterization described below were conducted in <b>2013-2016 by Evgeniy Shkondin, DTU Nanolab</b>.<br>
 
== Procces flow description ==


=====Si template fabrication=====
=====Si template fabrication=====
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=====Atomic Layer Deposition=====
=====Atomic Layer Deposition=====
The AZO coatings were made in a thermal, hot-wall ALD system (Picosun R200). The precursors were obtained from Strem Chemicals. ZnO was deposited using diethylzinc (Zn (C<sub>2</sub>H<sub>5</sub>)<sub>2</sub>, DEZ) and deionized water (H<sub>2</sub>O), whereas Al doping of the ZnO was introduced by a single cycle of trimethylaluminium (Al(CH<sub>3</sub>)<sub>3</sub>, TMA) and H<sub>2</sub>O into a ZnO matrix made by 20 cycles of “DEZ +H<sub>2</sub>O”. This defines an AZO macrocycle: 20 cycles of “DEZ+H<sub>2</sub>O” and one cycle of “TMA+H<sub>2</sub>O”. The deposition temperature was kept constant at 200°C. Approximately 55 AZO macrocycles need to be deposited in order to fill the Si trench template entirely.
The AZO coatings were made in a thermal, hot-wall ALD system (Picosun R200). The precursors were obtained from Strem Chemicals. ZnO was deposited using diethylzinc (Zn (C<sub>2</sub>H<sub>5</sub>)<sub>2</sub>, DEZ) and deionized water (H<sub>2</sub>O), whereas Al doping of the ZnO was introduced by a single cycle of trimethylaluminium (Al(CH<sub>3</sub>)<sub>3</sub>, TMA) and H<sub>2</sub>O into a ZnO matrix made by 20 cycles of “DEZ +H<sub>2</sub>O”. This defines an AZO macrocycle: 20 cycles of “DEZ+H<sub>2</sub>O” and one cycle of “TMA+H<sub>2</sub>O”. The deposition temperature was kept constant at 200°C. Approximately, 55 AZO macrocycles need to be deposited in order to fill the Si trench template entirely.


=====Top layer removal and selective etch of the Si template=====
=====Top layer removal and selective etch of the Si template=====
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|-
|-
!1.1
!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"
!1.2
!1.2
|DUV Resist patterning
|DUV Resist patterning.
|DUV
|DUV
|[[Specific_Process_Knowledge/Lithography/DUVStepperLithography|DUV Stepper Lithography]].  
|[[Specific_Process_Knowledge/Lithography/DUVStepperLithography|DUV Stepper Lithography]].  
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|-
|-
!1.3
!1.3
|Deep reactive ion etching (DRIE)
|Deep reactive ion etching (DRIE).
|DRIE; [[Specific_Process_Knowledge/Etch/DRIE-Pegasus/DUVetch|Recipe: PolySOI10]] Recipe needs to be tuned. Adjusted parameters: temperature, etching and passivation times.
|DRIE; [[Specific_Process_Knowledge/Etch/DRIE-Pegasus/DUVetch|Recipe: PolySOI10]] Recipe needs to be tuned. Adjusted parameters: temperature, etching and passivation times.
| [[Specific_Process_Knowledge/Etch/DRIE-Pegasus|DRIE Pegasus]].
| [[Specific_Process_Knowledge/Etch/DRIE-Pegasus|DRIE Pegasus]].
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|- style="background:#BCD4E6; color:black"
|- style="background:#BCD4E6; color:black"
!1.4
!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)
|
|
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|-
|-
!1.5
!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_1|SEM Supra 1]]  
[[Specific_Process_Knowledge/Characterization/SEM_Supra_1|SEM Supra 1]]  
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|- style="background:#BCD4E6; color:black"
|- style="background:#BCD4E6; color:black"
!1.6
!1.6
|Atomic Layer Deposition of Al-doped ZnO (AZO)
|Atomic Layer Deposition of Al-doped ZnO (AZO).
|Deposition carried at 200<sup>o</sup>C. Thickness is above 100 nm.
|Deposition carried at 200<sup>o</sup>C. Thickness is above 100 nm.
||Equipment used: [[Specific_Process_Knowledge/Thin_film_deposition/ALD_Picosun_R200|ALD Picosun R200]]. Standard recipe used: [[Specific_Process_Knowledge/Thin_film_deposition/ALD_Picosun_R200/AZO_deposition_using_ALD| AZO 20T]].
||Equipment used: [[Specific_Process_Knowledge/Thin_film_deposition/ALD_Picosun_R200|ALD Picosun R200]]. Standard recipe used: [[Specific_Process_Knowledge/Thin_film_deposition/ALD_Picosun_R200/AZO_deposition_using_ALD| AZO 20T]].
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|-
|-
!1.7
!1.7
|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_1|SEM Supra 1]]  
[[Specific_Process_Knowledge/Characterization/SEM_Supra_1|SEM Supra 1]]  
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|-
|-
!1.9
!1.9
|Scanning Electron Microscopy inspection
|Scanning Electron Microscopy inspection.
|By cleaving the sample it is possible to inspect IBE etching results in cross-sectional mode
|By cleaving the sample it is possible to inspect IBE etching results in cross-sectional mode.
|
|
[[Specific_Process_Knowledge/Characterization/SEM_Supra_1|SEM Supra 1]]  
[[Specific_Process_Knowledge/Characterization/SEM_Supra_1|SEM Supra 1]]  
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