Specific Process Knowledge/Thin film deposition/ALD2 (PEALD): Difference between revisions

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=ALD Picosun 200=
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=ALD 2 (PEALD)=


[[Category: Equipment|Thin film]]
[[Category: Equipment|Thin film]]
[[Category: Thin Film Deposition|ALD]]
[[Category: Thin Film Deposition|ALD]]


== ALD - Atomic layer deposition ==
[[image:ALD2.jpg|300x300px|right|thumb|Picosun R200 PEALD, positioned in cleanroom F-2.]]


The ALD2 (atomic layer deposition) tool from Picosun R200 with plasma capability is used to deposit a very thin layer of Al<sub>2</sub>O<sub>3</sub>, TiO<sub>2</sub> (amorphous or anatase), SiO<sub>2</sub>, HfO<sub>2</sub>, TiN and AlN.
== Thermal ALD and PEALD ==
[[image:ALD2.jpg|450x450px|right|thumb|ALD 2 (PEALD). Positioned in cleanroom F-2.]]
 
The ALD 2 (PEALD) is used to deposit very thin and uniform layers of different materials, by use of thermal ALD (Atomic Layer Deposition) or PEALD (Plasma Enhanced ALD). Layers can be up to 100 nm thick, see the table below.
 
The ALD deposition takes place in an ALD reactor chamber. In order to ensure that the temperature inside this reactor is the same everywhere, it has a dual chamber structure. The inner chamber is the reactor chamber, and the outer chamber is isolating the reactor chamber from room air. Both the inner and the outer chamber are under vacuum. The space between the two chambers is called an intermediate space (IMS), and the IMS is constantly purged with nitrogen.
 
When a sample is loaded into the reactor chamber, it will take some time before it reaches the desired temperature. Thus, it is important to include a temperature stabilization time in the deposition recipes.


Each process is using two different precurcors. The reaction takes place in cycles. During each cycle a very short pulse of each precursor is introduced into the ALD reaction chamber in turns, and in-between each precursor pulse the chamber is purged with nitrogen. All reactions have to take place on the sample surface, thus it is very important that each precurcor is removed from the chamber before the next one is introduced. In that way the ALD layer will be deposited atomic layer by atomic layer.  
The ALD depositions take place under vacuum, thus a vacuum pump is connected to the bottom of the ALD reactor chamber. The pump is located in the basement.


In order to ensure that the ALD reactor has the same temperature eveywhere, it has a dual chamber structure. The inner chamber is the ALD reactor with the sample holder, and the outer chamber is a vacuum chamber that is isolating the reactor from room air. The space between the two chambers is called an intermediate space (IMS). The IMS is connected to a nitrogen carrier gas line.  
Different precursor lines are connected to the reactor chamber through separate precursor inlets. At the moment the available precursors here are TMA, TiCl<sub>4</sub>, SAM24, TEMAHf, H<sub>2</sub>O and NH<sub>3</sub>, and soon O<sub>3</sub> will also be available. These precursor lines are all purged with a constant flow of nitrogen.  


When the reactor chamber is heated up or cooled down, it will take some time before the sample holder and the sample reach the desired temperature. Thus, it is important to include a temperature stabilization time in the process recipes.  
The liquid precursor sources TMA, TiCl<sub>4</sub> and H<sub>2</sub>O are stored in bottles located in a side cabinet on the left side of the machine. When the TMA and TiCl<sub>4</sub> precursors are not in use, a manual valve on each bottle has to be closed. The powder precursors SAM24 and TEMAHf are stored in bottles located in a big cabinet below the ALD chamber. These precursors are heated by heating jackets, and users should not open and close the manual valves. O<sub>3</sub> is generated by use of an ozone generator that is located in the E-rack at the right side of the machine.  


The ALD deposition takes place in the reactor chamber. All precursor and nitrogen carrier gas lines are connected to the reactor chamber through separate gas lines. The percursors pulse time is controlled using special ALD valves, that allow very short precursors pulses to be introduced into the ALD reactor and a at the same time allow a constant nitrogen purge.
A remote plasma generator is connected to the upper part of the reactor chamber. Different precursor gases are connected to this plasma generator through the same gas inlet. At the moment the available plasma precursor gases are N<sub>2</sub>, O<sub>2</sub>, NH<sub>3</sub> and H<sub>2</sub>. The plasma gas inlet is constantly purged with argon. The plasma gases can also be used as precursors for thermal ALD if the power to the plasma generator is not turned on. When H<sub>2</sub> is being used, the pump line constantly has to be purged with 1.9 SLM nitrogen, and this has to be enabled manually.


The ALD reaction takes place under vacuum, thus a vacuum pump is connected to the bottom of the ALD reactor. The pump is located in the basement.  
The plasma generator is separated from the reactor chamber by a plasma cone (or chamber lid). The argon flow through the plasma gas inlet ensures that the plasma cone remains clean.  


The liquid precursors (TMA, TiCl<sub>4</sub> and H<sub>2</sub>O) are located in the cabinet below the ALD chamber. When the TMA and TiCl<sub>4</sub> precursors are not in use, the manual valves have to be closed. Ozone is generated by use of an ozone generator that is located on the side of the machine.  
The plasma cone is not heated, and thus is will affect the temperature uniformity in the reactor chamber, and it will affect the gas flows and increase the necessary purge time. For that reason it is possible to mount a thermal lid between the plasma cone and the reactor chamber. However, it is quite time consuming to install the thermal lid as it requires that the machine is cooled to room temperature and vented. Furthermore, it is not possible to run plasma processes with the thermal lid installed.


It is possible to change the sample holder, so that ALD deposition can take place on different samples, e.g. a small wafer batch or a number of smaller samples. Samples are loaded manually into the sample holder by use of a tweezer.  
The precursor pulse time is controlled by special ALD valves that allow very short precursor pulses to be introduced into the ALD reactor chamber and at the same time allow a constant nitrogen or argon flow. Thus, nitrogen and argon are always flowing through the ALD valves into the chamber, independent on whether a precursor pulse is introduced or not.  


A short presentation with some information about the ALD tool can be found [[Media:ProcessMeeting ALD 2013-12-06_1.pdf|here]].
At the moment it is possible to deposit Al<sub>2</sub>O<sub>3</sub>, TiO<sub>2</sub>, HfO<sub>2</sub>, SiO<sub>2</sub>, AlN and TiN in the ALD. In order to deposit good quality nitride layers with low sheet resistance, the amount of oxygen has to be very low. Thus, the ALD reactor chamber has to be passivated for about three days, before nitride depositions can be done, and oxides and nitrides cannot be deposited at same time.
 
Samples are loaded through a load lock. 6" and 8" wafers can be loaded directly in the load lock, while 4" wafers and smaller samples have to be placed on a 6" carrier plate or a 6" silicon dummy wafer with an etched recess. It is only possible to load one wafer or carrier plate at a time by use of the load lock.
 
The plasma cone is opened and closed, when samples are transferred between the load lock and the reactor chamber. Two buttons on the load lock are used to insert and retract the load lock arm from the reactor chamber. A window on the front side of the machine makes it possible to keep an eye on the reactor chamber and the sample during loading and unloading. 
 
It is also possible to load a minibatch directly holder into ALD through a door on the left side of the reactor chamber. However, a training is needed in order to use the minibatch holder, and for nitride depositions the minibatch holder cannot be used as it requires that the machine is vented, and thus a possible nitride passivation will be ruined. Furthermore, the minibatch holder is not useful for plasma process, as the ALD material will only be deposited on the top sample.
 
The ALD is controlled by use of a computer with a touch screen that is situated next to the machine.
 
The ALD 2 (PEALD) is a Picosun R-200 Advanced Plasma ALD manufactured by Picosun, and it was installed in the cleanroom in 2016.  




'''The user manual, the user APV and contact information can be found in LabManager:'''
'''The user manual, the user APV and contact information can be found in LabManager:'''


[http://labmanager.danchip.dtu.dk/function.php?module=Machine&view=view&mach=321 ALD Picosun R200 info page in LabManager],
[http://labmanager.dtu.dk/function.php?module=Machine&view=view&mach=365 ALD 2 (PEALD) info page in LabManager]


== Process information ==
== Process information ==


*[[/Standard recipes on the ALD tool|Standard recipes on the ALD tool]]
'''Standard recipes on ALD 2 (PEALD):'''
*[[/ALD multilayers|Advanced recipes involving fabrication of multilayers]]
 
*[[/Al2O3 deposition using ALD|Al<sub>2</sub>O<sub>3</sub> deposition using ALD]]
*[[/Standard recipes on the ALD2 tool|Standard recipes on the <b>ALD 2 (PEALD)</b>]]
*[[/TiO2 deposition using ALD|TiO<sub>2</sub> deposition using ALD]]
 
 
'''Available processes:'''
 
*[[/Al2O3 deposition using ALD2| Al<sub>2</sub>O<sub>3</sub> deposition using '''ALD 2 (PEALD)''']]
 
*[[/TiO2 deposition using ALD2| TiO<sub>2</sub> deposition using '''ALD 2 (PEALD)''']]
 
*[[/HfO2 deposition using ALD2| HfO<sub>2</sub> deposition using '''ALD 2 (PEALD)''']]
 
*[[/SiO2 deposition using ALD2| SiO<sub>2</sub> deposition using '''ALD 2 (PEALD)''' - The process is obsolete]]
 
*[[/AlN deposition using ALD2| AlN deposition using '''ALD 2 (PEALD)''']]
 
*[[/TiN deposition using ALD2| TiN deposition using '''ALD 2 (PEALD)''']]
 
*[[/Al2O3 deposition using plasma ALD2 at room temperature| Al<sub>2</sub>O<sub>3</sub> deposition using '''ALD 2 (PEALD)''' at room temperature]]


==Equipment performance and process related parameters==
==Equipment performance and process related parameters==
Line 45: Line 77:


!colspan="2" border="none" style="background:silver; color:black;" align="center"|Equipment  
!colspan="2" border="none" style="background:silver; color:black;" align="center"|Equipment  
|style="background:WhiteSmoke; color:black"|<b>ALD2 (PEALD)</b>
|style="background:WhiteSmoke; color:black"|<b>ALD 2 (PEALD)</b>
|-
|-
!style="background:silver; color:black;" align="center" width="60"|Purpose  
!style="background:silver; color:black;" align="center" width="60"|Purpose  
|style="background:LightGrey; color:black"|ALD (atomic layer deposition) of
|style="background:LightGrey; color:black"|Thermal ALD or PEALD deposition
|style="background:WhiteSmoke; color:black"|
|style="background:WhiteSmoke; color:black"|
*Al<sub>2</sub>O<sub>3</sub>
*Al<sub>2</sub>O<sub>3</sub> - Thermal Al<sub>2</sub>O<sub>3</sub> (mainly backup for ALD1) and Al<sub>2</sub>O<sub>3</sub> using plasma
*TiO<sub>2</sub> (amorphous or anatase)
*TiO<sub>2</sub> (amorphous or anatase) - Thermal TiO<sub>2</sub> (mainly backup for ALD1) and TiO<sub>2</sub> using plasma
*SiO<sub>2</sub>
*HfO<sub>2</sub> - Thermal HfO<sub>2</sub> (mainly backup for ALD1)
*HfO<sub>2</sub>
*AlN - AlN using plasma
*TiN
*TiN - Thermal TiN and TiN using plamsa
*AlN
*ZnO
*AZO
All precursors might not be available at the same time.
Is is not possible to deposit oxides and nitrides at the same time.
|-
|-
!style="background:silver; color:black" align="center" valign="center" rowspan="2"|Performance
!style="background:silver; color:black" align="center" valign="center" rowspan="2"|Performance
|style="background:LightGrey; color:black"|Deposition rates
|style="background:LightGrey; color:black"|Deposition rates
|style="background:WhiteSmoke; color:black"|
|style="background:WhiteSmoke; color:black"|
*Al<sub>2</sub>O<sub>3</sub>: ~ 0.075 - 0.097 nm/cycle (Using the "Al2O3" recipe, depending on the temperature)
Depending on the deposited materials and temperature
*TiO<sub>2</sub>: 0.041 - 0.061 nm/cycle (Using the "TiO2" recipe, depending on the temperature)
More information can be found on the pages under "Process information"
|-
|-
|style="background:LightGrey; color:black"|Thickness
|style="background:LightGrey; color:black"|Thickness
|style="background:WhiteSmoke; color:black"|
|style="background:WhiteSmoke; color:black"|
*Al<sub>2</sub>O<sub>3</sub>: 0 - 100 nm
*Oxides: Al<sub>2</sub>O<sub>3</sub>, TiO<sub>2</sub>, HfO<sub>2</sub>, ZnO, AZO: 0-100 nm
*Nitrides: SiO<sub>2</sub>, AlN, TiN: 0-100 nm  
<i>As the purpose of ALD 2 is to deposit very thin and uniform layers, the allowed deposition thickness is limited to 100 nm, and it is not allowed to do more depositions on the same sample(s) to deposit thicker layers than 100 nm. Deposition of thicker layers is not allowed, because this will occupy the machine for long time and thus make it available for less users. Long depositions also cause issues and with flakes and particles, which means that the chamber and the pump line will have to be cleaned or changed quite often. Furthermore, the delivery time on precursors is usually quite long. So when you make a sample design, you should avoid steps, where you need to deposit thicker layers than 100 nm with ALD, or you can consider, if the same material can be deposited using other machines in the cleanroom.</i>
|-
!style="background:silver; color:black" align="center" valign="center" rowspan="3"|Process parameter
|style="background:LightGrey; color:black"|Deposition temperature
|style="background:WhiteSmoke; color:black"|
Maximum 500 <sup>o</sup>C
|-
|-
!style="background:silver; color:black" align="center" valign="center" rowspan="2"|Process parameter range
|style="background:LightGrey; color:black"|Thermal precursors
|style="background:LightGrey; color:black"|Temperature
|style="background:WhiteSmoke; color:black"|
|style="background:WhiteSmoke; color:black"|
*Al<sub>2</sub>O<sub>3</sub>: 150 - 350 <sup>o</sup>C
*TMA - Trimethylaluminium
*TiCl<sub>4</sub> - Titaniumtetrachloride
*H<sub>2</sub>O - Water
*O<sub>3</sub> - Ozone. Not available at the moment
*NH<sub>3</sub> - Ammonia
*SAM24 - Bis(diethylamono)silane
*TEMAHf - Tetrakis(ethylmethylamino)hafnium
|-
|-
|style="background:LightGrey; color:black"|Precursors
|style="background:LightGrey; color:black"|Plasma precursors
|style="background:WhiteSmoke; color:black"|
|style="background:WhiteSmoke; color:black"|
*TMA
*N<sub>2</sub>
*TiCl<sub>4</sub>
*H<sub>2</sub>O
*O<sub>3</sub>
*O<sub>2</sub>
*O<sub>2</sub>
*NH<sub>3</sub>
*H<sub>2</sub>
|-
|-
!style="background:silver; color:black" align="center" valign="center" rowspan="3"|Substrates
!style="background:silver; color:black" align="center" valign="center" rowspan="3"|Substrates
|style="background:LightGrey; color:black"|Batch size
|style="background:LightGrey; color:black"|Batch size
|style="background:WhiteSmoke; color:black"|
|style="background:WhiteSmoke; color:black"|
*Samples and single wafers are loaded through the load lock
*Smaller samples - Loaded on a 150 mm carrier plate or dummy wafer with an etched recess through the load lock
*100 mm and smaller are loaded on a carrier plate (150 mm)
*One 100 mm wafer - Loaded on a 150 mm carrier plate or dummy wafer with an etched recess through the load lock
*150 mm or 200 mm wafer don't need the carrier plate
*One 150 mm wafer - Loaded directly through the loadlock
*Up to 5 wafers when doing thermal ALD of oxides wafer size 100 mm, 150 mm and 200 mm
*One 200 mm wafer - Loaded directly through the loadlock
*For thermal ALD depositions of oxides, there is room for up to five wafers. 100, 150 and 200 mm wafers have to be loaded directly into the ALD chamber
|-
|-
| style="background:LightGrey; color:black"|Allowed materials
| style="background:LightGrey; color:black"|Allowed materials
Line 93: Line 140:
*Silicon oxide, silicon nitride
*Silicon oxide, silicon nitride
*Quartz/fused silica  
*Quartz/fused silica  
*Al, Al<sub>2</sub>O<sub>3</sub>
*Metals - Use a dedicated carrier wafer
*Ti, TiO<sub>2</sub>
*III-V materials - Use a dedicated carrier wafer
*Other metals (use dedicated carrier wafer)
*Polymers - Depending on the melting point/deposition temperature, use carrier wafer. Ask for permission
*III-V materials (use dedicated carrier wafer)
*Polymers (depending on the melting point/deposition temperature, use carrier wafer)
|-  
|-  
|}
|}

Latest revision as of 13:41, 15 August 2023

Feedback to this page: click here

This page is written by DTU Nanolab internal

ALD 2 (PEALD)


Thermal ALD and PEALD

ALD 2 (PEALD). Positioned in cleanroom F-2.

The ALD 2 (PEALD) is used to deposit very thin and uniform layers of different materials, by use of thermal ALD (Atomic Layer Deposition) or PEALD (Plasma Enhanced ALD). Layers can be up to 100 nm thick, see the table below.

The ALD deposition takes place in an ALD reactor chamber. In order to ensure that the temperature inside this reactor is the same everywhere, it has a dual chamber structure. The inner chamber is the reactor chamber, and the outer chamber is isolating the reactor chamber from room air. Both the inner and the outer chamber are under vacuum. The space between the two chambers is called an intermediate space (IMS), and the IMS is constantly purged with nitrogen.

When a sample is loaded into the reactor chamber, it will take some time before it reaches the desired temperature. Thus, it is important to include a temperature stabilization time in the deposition recipes.

The ALD depositions take place under vacuum, thus a vacuum pump is connected to the bottom of the ALD reactor chamber. The pump is located in the basement.

Different precursor lines are connected to the reactor chamber through separate precursor inlets. At the moment the available precursors here are TMA, TiCl4, SAM24, TEMAHf, H2O and NH3, and soon O3 will also be available. These precursor lines are all purged with a constant flow of nitrogen.

The liquid precursor sources TMA, TiCl4 and H2O are stored in bottles located in a side cabinet on the left side of the machine. When the TMA and TiCl4 precursors are not in use, a manual valve on each bottle has to be closed. The powder precursors SAM24 and TEMAHf are stored in bottles located in a big cabinet below the ALD chamber. These precursors are heated by heating jackets, and users should not open and close the manual valves. O3 is generated by use of an ozone generator that is located in the E-rack at the right side of the machine.

A remote plasma generator is connected to the upper part of the reactor chamber. Different precursor gases are connected to this plasma generator through the same gas inlet. At the moment the available plasma precursor gases are N2, O2, NH3 and H2. The plasma gas inlet is constantly purged with argon. The plasma gases can also be used as precursors for thermal ALD if the power to the plasma generator is not turned on. When H2 is being used, the pump line constantly has to be purged with 1.9 SLM nitrogen, and this has to be enabled manually.

The plasma generator is separated from the reactor chamber by a plasma cone (or chamber lid). The argon flow through the plasma gas inlet ensures that the plasma cone remains clean.

The plasma cone is not heated, and thus is will affect the temperature uniformity in the reactor chamber, and it will affect the gas flows and increase the necessary purge time. For that reason it is possible to mount a thermal lid between the plasma cone and the reactor chamber. However, it is quite time consuming to install the thermal lid as it requires that the machine is cooled to room temperature and vented. Furthermore, it is not possible to run plasma processes with the thermal lid installed.

The precursor pulse time is controlled by special ALD valves that allow very short precursor pulses to be introduced into the ALD reactor chamber and at the same time allow a constant nitrogen or argon flow. Thus, nitrogen and argon are always flowing through the ALD valves into the chamber, independent on whether a precursor pulse is introduced or not.

At the moment it is possible to deposit Al2O3, TiO2, HfO2, SiO2, AlN and TiN in the ALD. In order to deposit good quality nitride layers with low sheet resistance, the amount of oxygen has to be very low. Thus, the ALD reactor chamber has to be passivated for about three days, before nitride depositions can be done, and oxides and nitrides cannot be deposited at same time.

Samples are loaded through a load lock. 6" and 8" wafers can be loaded directly in the load lock, while 4" wafers and smaller samples have to be placed on a 6" carrier plate or a 6" silicon dummy wafer with an etched recess. It is only possible to load one wafer or carrier plate at a time by use of the load lock.

The plasma cone is opened and closed, when samples are transferred between the load lock and the reactor chamber. Two buttons on the load lock are used to insert and retract the load lock arm from the reactor chamber. A window on the front side of the machine makes it possible to keep an eye on the reactor chamber and the sample during loading and unloading.

It is also possible to load a minibatch directly holder into ALD through a door on the left side of the reactor chamber. However, a training is needed in order to use the minibatch holder, and for nitride depositions the minibatch holder cannot be used as it requires that the machine is vented, and thus a possible nitride passivation will be ruined. Furthermore, the minibatch holder is not useful for plasma process, as the ALD material will only be deposited on the top sample.

The ALD is controlled by use of a computer with a touch screen that is situated next to the machine.

The ALD 2 (PEALD) is a Picosun R-200 Advanced Plasma ALD manufactured by Picosun, and it was installed in the cleanroom in 2016.


The user manual, the user APV and contact information can be found in LabManager:

ALD 2 (PEALD) info page in LabManager

Process information

Standard recipes on ALD 2 (PEALD):


Available processes:

Equipment performance and process related parameters

Equipment ALD 2 (PEALD)
Purpose Thermal ALD or PEALD deposition
  • Al2O3 - Thermal Al2O3 (mainly backup for ALD1) and Al2O3 using plasma
  • TiO2 (amorphous or anatase) - Thermal TiO2 (mainly backup for ALD1) and TiO2 using plasma
  • HfO2 - Thermal HfO2 (mainly backup for ALD1)
  • AlN - AlN using plasma
  • TiN - Thermal TiN and TiN using plamsa
  • ZnO
  • AZO

All precursors might not be available at the same time. Is is not possible to deposit oxides and nitrides at the same time.

Performance Deposition rates

Depending on the deposited materials and temperature. More information can be found on the pages under "Process information"

Thickness
  • Oxides: Al2O3, TiO2, HfO2, ZnO, AZO: 0-100 nm
  • Nitrides: SiO2, AlN, TiN: 0-100 nm

As the purpose of ALD 2 is to deposit very thin and uniform layers, the allowed deposition thickness is limited to 100 nm, and it is not allowed to do more depositions on the same sample(s) to deposit thicker layers than 100 nm. Deposition of thicker layers is not allowed, because this will occupy the machine for long time and thus make it available for less users. Long depositions also cause issues and with flakes and particles, which means that the chamber and the pump line will have to be cleaned or changed quite often. Furthermore, the delivery time on precursors is usually quite long. So when you make a sample design, you should avoid steps, where you need to deposit thicker layers than 100 nm with ALD, or you can consider, if the same material can be deposited using other machines in the cleanroom.

Process parameter Deposition temperature

Maximum 500 oC

Thermal precursors
  • TMA - Trimethylaluminium
  • TiCl4 - Titaniumtetrachloride
  • H2O - Water
  • O3 - Ozone. Not available at the moment
  • NH3 - Ammonia
  • SAM24 - Bis(diethylamono)silane
  • TEMAHf - Tetrakis(ethylmethylamino)hafnium
Plasma precursors
  • N2
  • O2
  • NH3
  • H2
Substrates Batch size
  • Smaller samples - Loaded on a 150 mm carrier plate or dummy wafer with an etched recess through the load lock
  • One 100 mm wafer - Loaded on a 150 mm carrier plate or dummy wafer with an etched recess through the load lock
  • One 150 mm wafer - Loaded directly through the loadlock
  • One 200 mm wafer - Loaded directly through the loadlock
  • For thermal ALD depositions of oxides, there is room for up to five wafers. 100, 150 and 200 mm wafers have to be loaded directly into the ALD chamber
Allowed materials
  • Silicon
  • Silicon oxide, silicon nitride
  • Quartz/fused silica
  • Metals - Use a dedicated carrier wafer
  • III-V materials - Use a dedicated carrier wafer
  • Polymers - Depending on the melting point/deposition temperature, use carrier wafer. Ask for permission