Specific Process Knowledge/Thin film deposition/ALD Picosun R200/ZnO deposition using ALD: Difference between revisions

From LabAdviser
Jump to navigation Jump to search
(Created page with "ZnO")
 
No edit summary
Line 1: Line 1:
ZnO
The ALD window for deposition of zinc oxide (ZnO) ranges from 100 <sup>o</sup>C to 250 <sup>o</sup>C. Several investigation techniques has been implemented for ZnO characterization. Additionally, more information on ZnO can be found on a page about [[Specific_Process_Knowledge/Thin_film_deposition/ALD_Picosun_R200/AZO_deposition_using_ALD|Al-doped ZnO (AZO)]]
 
All results shown on this page have been obtained using the "ZnOT" recipe on new Si(100) wafers with native oxide:
 
==Al<sub>2</sub>O<sub>3</sub> standard recipe==
 
<b>Recipe: AL2O3</b>
 
<b>Maximum deposition thickness: 100 nm</b>
 
<b>Temperature: 100 <sup>o</sup>C - 350 <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
|0.1 s
|-
!Purge time
|3.0 s
|4.0 s
|-
|}
 
This is the standard recipe for deposition of Al<sub>2</sub>O<sub>3</sub> on flat and high aspect ratio structures. For conformal passivation of porous materials, very narrow trenches etc. it is recomanded to use <b>Al2O3T</b> recipe instead. Recipe can be used for deposition in the range 100-350 <sup>o</sup>C. However, at 100 <sup>o</sup>C small amount of carbon impurities has been observed. It is not recomanded to use this recipe for deposition below 100 <sup>o</sup>C, since it also leads to accumulation of H<sub>2</sub>O in the chamber.
 
===Al<sub>2</sub>O<sub>3</sub> deposition rates===
 
The deposition rate for Al<sub>2</sub>O<sub>3</sub> depends on the temperature, see the ALD-window graph below.  The uniformity, thickness, refractive index has been obtained using [[Specific_Process_Knowledge/Characterization/Optical_characterization#Ellipsometer|Ellipsometer VASE]].
 
 
<gallery caption="" widths="500px" heights="500px" perrow="2">
image:ALD_window.jpg| ALD-window for Al<sub>2</sub>O<sub>3</sub> deposition.
image:SE_Al2O3_ALD_typical.JPG| Typical uniformity profile across 100mm Si wafer based on 49 mesurement points.
</gallery>
 
In the graphs below the Al<sub>2</sub>O<sub>3</sub> thickness as function of number of cycles for deposition temperatures between 100 <sup>o</sup>C and 350 <sup>o</sup>C can be seen. From the equations the number of cycles required for a certain thickess can be calculated.
 
 
 
<gallery caption="Aluminium oxide thickness as function of number of cycles" widths="500px" heights="500px" perrow="3">
image:Al2O3 100C.jpg| Temperature 100 <sup>o</sup>C.
image:Al2O3 150C.jpg| Temperature 150 <sup>o</sup>C.
image:Al2O3 200C.jpg| Temperature 200 <sup>o</sup>C.
</gallery>
 
<gallery caption="Aluminium oxide thickness as function of number of cycles" widths="500px" heights="500px" perrow="3">
image:Al2O3 250C.jpg| Temperature 250 <sup>o</sup>C.
image:Al2O3 300C.jpg| Temperature 300 <sup>o</sup>C.
image:Al2O3 350C.jpg| Temperature 350 <sup>o</sup>C.
</gallery>
 
<br clear="all" />
<b>Evgeniy Shkondin, DTU Danchip, 2014-2016.</b>
<br clear="all" />
<br clear="all" />
 
===Al<sub>2</sub>O<sub>3</sub> standard recipe characterization across 100 mm Si <100> wafer ===
 
 
 
 
{| border="2" cellspacing="2" cellpadding="3" colspan="10"
|bgcolor="#98FB98" |'''Al<sub>2</sub>O<sub>3</sub> deposition at 100 <sup>o</sup>C and 150 <sup>o</sup>C'''
|-
|
 
 
{| {{table}}
| align="center" |
{| border="2" cellspacing="2" cellpadding="3"  align="center" style="width:750px"
! colspan="5" |Deposition conditions at 100 <sup>o</sup>C
|-
!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>
 
|-
|150
|14.11
|2.18
|0.225
|1.56
 
|-
|300
|25.94
|0.68
|0.14
|1.59
 
|-
|500
|41.35
|1.87
|0.60
|1.59
 
|-
|800
|65.05
|2.28
|1.13
|1.59
 
|-
|1088
|87.25
|2.15
|1.35
|1.60
 
|-
|}
 
 
| align="center" valign="top"|
{| border="2" cellspacing="2" cellpadding="3" align="center" style="width:750px"
! colspan="5" |Deposition conditions at 150 <sup>o</sup>C
|-
!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>
 
|-
|150
|15.38
|1.72
|0.18
|1.61
 
|-
|300
|28.67
|1.73
|0.36
|1.62
 
|-
|500
|46.93
|1.75
|0.57
|1.62
 
|-
|800
|73.46
|1.75
|0.92
|1.63
 
|-
|1088
|99.50
|1.74
|1.20
|1.63
 
|-
|}
|-
|}
|}
 
%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%
 
 
{| border="2" cellspacing="2" cellpadding="3" colspan="10"
|bgcolor="#98FB98" |'''Al<sub>2</sub>O<sub>3</sub> deposition at 200 <sup>o</sup>C and 250 <sup>o</sup>C'''
|-
|
 
 
{| {{table}}
| align="center" |
{| border="2" cellspacing="2" cellpadding="3"  align="center" style="width:750px"
! colspan="5" |Deposition conditions at 200 <sup>o</sup>C
|-
!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>
 
|-
|150
|16.46
|2.92
|0.33
|1.62
 
|-
|300
|31.09
|1.53
|0.34
|1.63
 
|-
|500
|51.20
|1.10
|0.39
|1.64
 
|-
|800
|79.66
|1.59
|0.88
|1.64
 
|-
|1088
|107.69
|1.41
|1.04
|1.64
 
|-
|}
 
 
| align="center" valign="top"|
{| border="2" cellspacing="2" cellpadding="3" align="center" style="width:750px"
! colspan="5" |Deposition conditions at 250 <sup>o</sup>C
|-
!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>
 
|-
|150
|16.41
|0.83
|0.10
|1.63
 
|-
|300
|30.81
|1.13
|0.24
|1.64
 
|-
|500
|50.48
|1.10
|0.40
|1.64
 
|-
|800
|79.84
|1.11
|0.60
|1.65
 
|-
|1088
|108.03
|1.11
|0.61
|1.65
 
|-
|}
|-
|}
|}
%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%
 
 
{| border="2" cellspacing="2" cellpadding="3" colspan="10"
|bgcolor="#98FB98" |'''Al<sub>2</sub>O<sub>3</sub> deposition at 300 <sup>o</sup>C and 350 <sup>o</sup>C'''
|-
|
 
 
{| {{table}}
| align="center" |
{| border="2" cellspacing="2" cellpadding="3"  align="center" style="width:750px"
! colspan="5" |Deposition conditions at 300 <sup>o</sup>C
|-
!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>
 
|-
|150
|15.59
|2.11
|0.24
|1.63
 
|-
|300
|29.00
|0.79
|0.17
|1.65
 
|-
|500
|47.86
|1.71
|0.26
|1.64
 
|-
|800
|75.04
|0.90
|0.55
|1.65
 
|-
|1088
|101.76
|0.75
|0.62
|1.65
 
|-
|}
 
 
| align="center" valign="top"|
{| border="2" cellspacing="2" cellpadding="3" align="center" style="width:750px"
! colspan="5" |Deposition conditions at 350 <sup>o</sup>C
|-
!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>
 
|-
|150
|13.88
|0.69
|0.06
|1.67
 
|-
|300
|26.70
|0.62
|0.12
|1.64
 
|-
|500
|43.70
|0.42
|0.15
|1.64
 
|-
|800
|68.77
|0.65
|0.37
|1.65
 
|-
|1088
|92.88
|0.70
|0.48
|1.66
 
|-
|}
|-
|}
|}
 
<br clear="all" />
<b>Evgeniy Shkondin, DTU Danchip, 2014-2016.</b>
<br clear="all" />
<br clear="all" />
 
===Al<sub>2</sub>O<sub>3</sub> XPS investigation for elemental trace analysis===
 
XPS profile for Al<sub>2</sub>O<sub>3</sub> has been obtained using [[Specific_Process_Knowledge/Characterization/XPS#XPS-ThermoScientific|XPS-ThermoScientific]]. Al<sub>2</sub>O<sub>3</sub> samples reveals chemically high quality films with no observable contaminations in temperature range 150 - 350 <sup>o</sup>C. At lower temperature (100 <sup>o</sup>C) the ALD reaction starts to become unsufficient and some amount of carbon from TMA precursor gets absorbed into the film.
 
 
<gallery caption="" widths="500px" heights="500px" perrow="3">
image:Al2O3_XPS.jpg| Survey scan of Al<sub>2</sub>O<sub>3</sub>.
image:LT_Al2O3_Carbon_content.JPG| <b>C 1s</b> scan of Al<sub>2</sub>O<sub>3</sub> film deposited at 100<sup>o</sup>C. Shows clearly carbon impurities in the film
image:HT_Al2O3_Carbon_content.JPG| <b>C 1s</b> scan of Al<sub>2</sub>O<sub>3</sub> film deposited between 150<sup>o</sup>C - 350<sup>o</sup>C. No carbon observes.
</gallery>
 
<br clear="all" />
<b>Evgeniy Shkondin, DTU Danchip, 2014-2016.</b>
<br clear="all" />
<br clear="all" />

Revision as of 19:38, 16 March 2017

The ALD window for deposition of zinc oxide (ZnO) ranges from 100 oC to 250 oC. Several investigation techniques has been implemented for ZnO characterization. Additionally, more information on ZnO can be found on a page about Al-doped ZnO (AZO)

All results shown on this page have been obtained using the "ZnOT" recipe on new Si(100) wafers with native oxide:

Al2O3 standard recipe

Recipe: AL2O3

Maximum deposition thickness: 100 nm

Temperature: 100 oC - 350 oC

TMA H2O
Nitrogen flow 150 sccm 200 sccm
Pulse time 0.1 s 0.1 s
Purge time 3.0 s 4.0 s

This is the standard recipe for deposition of Al2O3 on flat and high aspect ratio structures. For conformal passivation of porous materials, very narrow trenches etc. it is recomanded to use Al2O3T recipe instead. Recipe can be used for deposition in the range 100-350 oC. However, at 100 oC small amount of carbon impurities has been observed. It is not recomanded to use this recipe for deposition below 100 oC, since it also leads to accumulation of H2O in the chamber.

Al2O3 deposition rates

The deposition rate for Al2O3 depends on the temperature, see the ALD-window graph below. The uniformity, thickness, refractive index has been obtained using Ellipsometer VASE.


In the graphs below the Al2O3 thickness as function of number of cycles for deposition temperatures between 100 oC and 350 oC can be seen. From the equations the number of cycles required for a certain thickess can be calculated.



Evgeniy Shkondin, DTU Danchip, 2014-2016.

Al2O3 standard recipe characterization across 100 mm Si <100> wafer

Al2O3 deposition at 100 oC and 150 oC


Deposition conditions at 100 oC
Number of cycles Thickness (nm) Uniformity across 100mm Si substrate (%) Standard deviation error Refractive index @ 632.8 nm
150 14.11 2.18 0.225 1.56
300 25.94 0.68 0.14 1.59
500 41.35 1.87 0.60 1.59
800 65.05 2.28 1.13 1.59
1088 87.25 2.15 1.35 1.60


Deposition conditions at 150 oC
Number of cycles Thickness (nm) Uniformity across 100mm Si substrate (%) Standard deviation error Refractive index @ 632.8 nm
150 15.38 1.72 0.18 1.61
300 28.67 1.73 0.36 1.62
500 46.93 1.75 0.57 1.62
800 73.46 1.75 0.92 1.63
1088 99.50 1.74 1.20 1.63

%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%


Al2O3 deposition at 200 oC and 250 oC


Deposition conditions at 200 oC
Number of cycles Thickness (nm) Uniformity across 100mm Si substrate (%) Standard deviation error Refractive index @ 632.8 nm
150 16.46 2.92 0.33 1.62
300 31.09 1.53 0.34 1.63
500 51.20 1.10 0.39 1.64
800 79.66 1.59 0.88 1.64
1088 107.69 1.41 1.04 1.64


Deposition conditions at 250 oC
Number of cycles Thickness (nm) Uniformity across 100mm Si substrate (%) Standard deviation error Refractive index @ 632.8 nm
150 16.41 0.83 0.10 1.63
300 30.81 1.13 0.24 1.64
500 50.48 1.10 0.40 1.64
800 79.84 1.11 0.60 1.65
1088 108.03 1.11 0.61 1.65

%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%%


Al2O3 deposition at 300 oC and 350 oC


Deposition conditions at 300 oC
Number of cycles Thickness (nm) Uniformity across 100mm Si substrate (%) Standard deviation error Refractive index @ 632.8 nm
150 15.59 2.11 0.24 1.63
300 29.00 0.79 0.17 1.65
500 47.86 1.71 0.26 1.64
800 75.04 0.90 0.55 1.65
1088 101.76 0.75 0.62 1.65


Deposition conditions at 350 oC
Number of cycles Thickness (nm) Uniformity across 100mm Si substrate (%) Standard deviation error Refractive index @ 632.8 nm
150 13.88 0.69 0.06 1.67
300 26.70 0.62 0.12 1.64
500 43.70 0.42 0.15 1.64
800 68.77 0.65 0.37 1.65
1088 92.88 0.70 0.48 1.66


Evgeniy Shkondin, DTU Danchip, 2014-2016.

Al2O3 XPS investigation for elemental trace analysis

XPS profile for Al2O3 has been obtained using XPS-ThermoScientific. Al2O3 samples reveals chemically high quality films with no observable contaminations in temperature range 150 - 350 oC. At lower temperature (100 oC) the ALD reaction starts to become unsufficient and some amount of carbon from TMA precursor gets absorbed into the film.



Evgeniy Shkondin, DTU Danchip, 2014-2016.