View source for Specific Process Knowledge/Thin film deposition/ALD Picosun R200/HfO2 deposition using ALD

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<b>Important</b>: The recipes and results listed on this page have been made in 2017. Updated results and recipes from 2019 can be found [[Specific_Process_Knowledge/Thin film deposition/ALD_Picosun R200/HfO2 deposition using ALD new page|<b>here</b>]]. 

The ALD temperature window for HfO2 is 150 - 300 <sup>o</sup>C. 

The TEMAHf precursor is heated to 125 <sup>o</sup>C (TE210) and the heater (TE211 max.) is set to 140 <sup>o</sup>C during deposition. Remember to set the values in the "MANUAL" tab and to change them to back after deposition (TE211 max. to 1 <sup>o</sup>C).  These values may not be exceeded to prevent precursor decomposition. Due to the heating of the precursor the '''stabilization time needs to be set to 60 min'''. Else an alarm (TE210 PID limit exceeded while pulsing) will be triggered and the process will be stopped after the first pulsing attempt.   


=HfO<sub>2</sub> standard recipe=

==HfO<sub>2</sub> deposition using TEMAHf and H<sub>2</sub>O precursors== <!-- 20170424A -->


The following tables show the recipe and boost settings for the TEMAHf precursor: 
{| border="2" cellspacing="2" cellpadding="5"  align="none"
|- 
|
!TEMAHf
!H<sub>2</sub>O
|-
!Nitrogen flow
|150 sccm
|120 sccm
|-
!Pulse time
|1.6 s
|0.1 s
|- 
!Purge time	
|8.0 s
|4.0 s
|-
|}


{| border="2" cellspacing="2" cellpadding="5"  align="none"

!Boost flow
|500 sccm
|-
!Pre-empty
|0.5 s
|-
!Master fill
|1.2 s
|- 
!Post-empty	
|0 s
|-
|}


===HfO<sub>2</sub> deposition at 150 <sup>o</sup>C===


Two HfO<sub>2</sub> depositions were made January 2018 - One for 91 cycles and one for 250 cycles. Both deposition were done on 4" wafers with native oxide. The deposition temperature was 150 <sup>o</sup>C , and the precursor temperature (T210) for TEMAHf was 125 <sup>o</sup>C.


'''Number of cycles: 91'''

''Results:''

Average HfO<sub>2</sub> thickness: 9.57 nm (measured in nine points)<br/> 
Deposition rate: 0.11 nm/cycle<br/> 
Non-uniformity: 4.15 %<br/> 

<gallery caption="" widths="450px" heights="450px" perrow="1"> 
image:150C91cycles.png| Ellipsometer measurement of HfO<sub>2</sub>. Deposition temperature: 150 <sup>o</sup>C. Number of cycles: 91.
</gallery>

'''Number of cycles: 250'''

''Results:''

Average HfO<sub>2</sub> thickness: 27.65 nm (measured in five points)<br/> 
Deposition rate: 0.11 nm/cycle<br/> 
Non-uniformity: 2,20 %<br/> 

<gallery caption="" widths="450px" heights="450px" perrow="1"> 
image:150C250cycles.png| Ellipsometer measurement of HfO<sub>2</sub>. Deposition temperature: 150 <sup>o</sup>C. Number of cycles: 250.
</gallery>

===HfO<sub>2</sub> deposition at 250 <sup>o</sup>C===

The test was done with 300 cycles at 250 <sup>o</sup>C where the deposition rate was measured to be '''0.0827 nm/cycle'''. The precursor temperature (T210) for TEMAHf was 125 <sup>o</sup>C.


<gallery caption="" widths="450px" heights="450px" perrow="1">
image:‎20170424A.png| Ellipsometer measurement of HfO<sub>2</sub>. Deposition temperature: 250 <sup>o</sup>C. Number of cycles: 300. 
</gallery>

{| border="2" cellspacing="2" cellpadding="5"  align="none"
!Parameter
!Average
!Min.
!Max.
!Std.Dev
!%Range
|-
!Thickness (nm)
|24.83
|24.05
|27.13
|0.68
|12.38
|}


<gallery caption="" widths="350px" heights="350px" perrow="2"> 
image:20170424AAFM.png| AFM measurement roughness 0.3784 nm.
</gallery>

The XPS measurement was made by our [[Specific_Process_Knowledge/Characterization/XPS/K-Alpha|XPS K-Alpha]] and shows that the film is purely  HfO<sub>2</sub> except for some impurities on the surface. 


<gallery caption="" widths="350px" heights="350px" perrow="2"> 
image:20170424AXPS.png| Atomic percentage distribution of a depth profile. 
</gallery>

<b>Tanja Amport, Pernille Voss Larsen and Mikkel Dysseholm Mar, DTU Nanolab (former DTU Danchip), 2017.</b>