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This page describes non standartv Al2O3 and tiO2 processes including multilayers structures
{{cc-nanolab}}
 
'''Feedback to this page''': '''[mailto:labadviser@nanolab.dtu.dk?Subject=Feed%20back%20from%20page%20https://labadviser.nanolab.dtu.dk//index.php?title=Specific_Process_Knowledge/Thin_film_deposition/ALD_Picosun_R200/ALD_multilayers click here]''' 
<br>
<br>
This page describes non-standart recipes including multilayers structures. They were the first test recipes on the ALD-1 to test the tool functionality and can be used as inspiration.
<br>
<br>
==Low temperature deposition of Al<sub>2</sub>O<sub>3</sub>==
 
<b>Recipe: Al2O3 LT</b>
 
<b>Temperature: 80-150 <sup>o</sup>C</b>
 
{| border="2" cellspacing="2" cellpadding="5"  align="none"
|-
|
!TMA
!H<sub>2</sub>O
|-
!Nitrogen flow
|150 sccm
|200 sccm
|-
!Pulse time
|0.1 s
|0.2 s
|-
!Purge time
|5.0 s
|10.0 s
|-
|}
 
Deposition rate: <b>0.089 nm/cycle </b>(@120 <sup>o</sup>C)
 
This recipe has been developd for fabrication of high quality homogenious optical layers at low temperature. Research related results with this recipe can be found here: [http://journals.aps.org/prl/abstract/10.1103/PhysRevLett.115.177402 LINK - requires login] (Phys. Rev. Lett. 115(17) 2015, 177402)
 
 
{| border="2" cellspacing="2" cellpadding="3" colspan="10"
|bgcolor="#98FB98" |'''Al<sub>2</sub>O<sub>3</sub> deposition at 120 <sup>o</sup>C'''
|-
|
 
 
{| {{table}}
| align="center" |
{| border="2" cellspacing="2" cellpadding="3"  align="center" style="width:750px"
! colspan="5" |Deposition conditions at 120 <sup>o</sup>C for Al2O3 LT recipe
|-
!Number of cycles
|<b>Thickness (nm)</b>
|<b>Uniformity across 100mm Si substrate (%)</b>
|<b>Standard deviation error</b>
|<b>Refractive index @ 632.8 nm</b>
 
|-
|250
|24.83
|1.22
|0.16
|1.61
 
|-
|500
|45.48
|1.35
|0.41
|1.63
 
|-
|750
|68.03
|1.42
|0.59
|1.63
 
|-
|1000
|90.66
|1.74
|0.94
|1.63
 
|-
|}
 
|-
|}
|}
 
 
 
The uniformity, thickness, refractive index has been obtained using [[Specific_Process_Knowledge/Characterization/Optical_characterization#Ellipsometer|Ellipsometer VASE]].
 
 
<gallery caption="" widths="400px" heights="350px" perrow="2">
image:Al2O3_LT_Thickness.JPG| Measured thickness distribution across 100 mm wafer.
image:Al2O3_LT_RI.JPG| Measured refractive index distribution across 100 mm wafer.
</gallery>
 
<br clear="all" />
<b>Evgeniy Shkondin, DTU Nanolab, 2014-2016.</b>
<br clear="all" />
<br clear="all" />
 
==Low temperature deposition of TiO<sub>2</sub>==
 
<b>Recipe: TiO2 LT</b>
 
<b>Temperature: 80-150 <sup>o</sup>C</b>
 
{| border="2" cellspacing="2" cellpadding="5"  align="none"
|-
|
!TiCl<sub>4</sub>
!H<sub>2</sub>O
|-
!Nitrogen flow
|150 sccm
|200 sccm
|-
!Pulse time
|0.2 s
|0.2 s
|-
!Purge time
|10.0 s
|15.0 s
|-
|}
 
Deposition rate: <b>0.048 nm/cycle </b>(@ 120 <sup>o</sup>C)
 
This recipe has been developd for fabrication of high quality homogenious optical layers at low temperature. The deposited TiO<sub>2</sub> layers are amorphous. Research related results with this recipe can be found here: [http://journals.aps.org/prl/abstract/10.1103/PhysRevLett.115.177402 LINK - requires longin] (Phys. Rev. Lett. 115(17) 2015, 177402)
 
 
{| border="2" cellspacing="2" cellpadding="3" colspan="10"
|bgcolor="#98FB98" |'''TiO<sub>2</sub> deposition at 120 <sup>o</sup>C'''
|-
|
 
 
{| {{table}}
| align="center" |
{| border="2" cellspacing="2" cellpadding="3"  align="center" style="width:750px"
! colspan="5" |Deposition conditions at 120 <sup>o</sup>C for TiO2 LT recipe
|-
!Number of cycles
|<b>Thickness (nm)</b>
|<b>Uniformity across 100mm Si substrate (%)</b>
|<b>Standard deviation error</b>
|<b>Refractive index @ 632.8 nm</b>
 
|-
|250
|10.17
|2.19
|0.14
|2.18
 
|-
|500
|23.12
|1.80
|0.23
|2.40
 
|-
|750
|34.13
|1.87
|0.39
|2.39
 
|-
|1000
|46.13
|1.78
|0.50
|2.39
 
|-
|}
 
|-
|}
|}
 
%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%
 
The uniformity, thickness, refractive index has been obtained using [[Specific_Process_Knowledge/Characterization/Optical_characterization#Ellipsometer|Ellipsometer VASE]].
 
 
<gallery caption="" widths="400px" heights="350px" perrow="2">
image:TiO2_LT_Thickness.JPG| Measured thickness distribution across 100 mm wafer.
image:TiO2_LT_RI.JPG| Measured refractive index distribution across 100 mm wafer.
</gallery>
 
<br clear="all" />
<b>Evgeniy Shkondin, DTU Nanolab, 2014-2016.</b>
<br clear="all" />
<br clear="all" />
 
==Low temperature grown multilayers on flat surfaces==
 
<b>Recipe: EMA01</b>
 
<b>Recipe: EMA02</b>
 
<b>Recipe: EMA03</b>
 
<b>Recipe: EMA04</b>
 
<b>Temperature: 120 <sup>o</sup>C</b>
 
All four recipes is based on <b>Al2O3_LT</b> amd <b>TiO2_LT</b> above mentioned low temperature recipes. Optical research based on fabricated Al<sub>2</sub>O<sub>3</sub> and TiO<sub>2</sub> multilayers has been published [http://journals.aps.org/prl/abstract/10.1103/PhysRevLett.115.177402 LINK] (Phys. Rev. Lett. 115(17) 2015, 177402)
 
 
<gallery caption="" widths="1000px" heights="700px" perrow="1">
image:multilayers222.jpg| Al<sub>2</sub>O<sub>3</sub>/TiO<sub>2</sub> multilayers.
</gallery>
 
<br clear="all" />
<b>Evgeniy Shkondin, DTU Nanolab (former DTU Danchip), 2014-2016.</b>
<br clear="all" />
<br clear="all" />
 
 
===Investigation of chemical composition in multilayers system===
 
Chemical tace analysis has been performed using [[Specific_Process_Knowledge/Characterization/XPS/K-Alpha|XPS K-Alpha]] equipment in depth profile mode.
 
<gallery caption="" widths="1000px" heights="1000px" perrow="1">
image:XPS_depth_multi_survey.JPG| Survey scan.
</gallery>
 
<br clear="all" />
 
<gallery caption="" widths="400px" heights="350px" perrow="2">
image:XPS_depth_Al_10_AL.jpg| Al 2p signal multilayers.
image:XPS_depth_Al_10_Ti.jpg| Ti 2p signal  multilayers.
image:XPS_depth_Al_10_O.jpg| O 1s signal  multilayers.
image:XPS_depth_Al_10_Si.jpg| Si 2p signal  multilayers.
</gallery>
 
<br clear="all" />
<b>Evgeniy Shkondin, DTU Nanolab (former DTU Danchip), 2014-2016.</b>
<br clear="all" />
<br clear="all" />
 
==Al<sub>2</sub>O<sub>3</sub>/TiO<sub>2</sub> multilayers on high aspect ratio structures==
 
<b>Recipe: Multi T</b>
 
<b>Temperature: 150 <sup>o</sup>C</b>
 
 
<gallery caption="" widths="1000px" heights="1000px" perrow="1">
image:Evgeniy Shkondin Si trenches coverd with Al2O3 and TiO2 multilayers using ALD.JPG| Al<sub>2</sub>O<sub>3</sub>/TiO<sub>2</sub> multilayers grown on silicon trenches.
 
</gallery>
 
 
<br clear="all" />
<b>Evgeniy Shkondin, DTU Nanolab (former DTU Danchip), 2014-2016.</b>
<br clear="all" />
<br clear="all" />
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