Jump to content

Specific Process Knowledge/Etch/Wet III-V Etches: Difference between revisions

Bghe (talk | contribs)
No edit summary
Jehan (talk | contribs)
 
(43 intermediate revisions by 6 users not shown)
Line 1: Line 1:
'''Feedback to this page''': '''[mailto:danchipsupport@danchip.dtu.dk?Subject=Feed%20back%20from%20page%20http://http://labadviser.danchip.dtu.dk/index.php?title=Specific_Process_Knowledge/Etch/Wet_III-V_Etches click here]'''  
'''Unless anything else is stated, everything on this page, text and pictures are made by DTU Nanolab.'''


This is a collection of III-V wet-etches; not all etches are currently used at DTU Danchip why the rates should be tested before use. Make sure you have the proper education in mixing of chemicals before use.
'''All links to Kemibrug (SDS) and Labmanager Including APV and QC requires login.'''


It is utterly important that you dispose of chemicals/etches according to the DTU Danchip regulations; more information is found in the III-V cleanroom.
'''Feedback to this page''': '''[mailto:labadviser@nanolab.dtu.dk?Subject=Feed%20back%20from%20page%20http://labadviser.nanolab.dtu.dk/index.php?title=Specific_Process_Knowledge/Etch/Wet_III-V_Etches click here]'''


This is a collection of III-V wet-etches; the rates should be tested before use. Make sure you have the proper education in mixing of chemicals before use. Wet etching of III-V materials is primarily to be done in 'Fume hood 07: III-V acids/bases'. Contact information, risk assessment and manual regarding this fume hood can be found in LabManager:
[http://labmanager.dtu.dk/function.php?module=Machine&view=view&mach=374 Fume hood 07 Info page in LabManager]
<br>
It is very important that you dispose off chemicals and process waste according to DTU Nanolab regulations and risk assessments for your work.
[[Image:FH07.jpg|300x300px|right|thumb|'Fume hood 07' in cleanroom D3]]
<br>
For dry etching III-V materials see
*[[Specific Process Knowledge/Etch/III-V ICP|III-V ICP]]
*[[Specific Process Knowledge/Etch/III-V RIE|III-V RIE - Plassys]] (will be decommissioned October 2025)
== InP substrate etching ==
When etching InP substrates, both 2” wafers and small pieces, you should collect the used chemicals in a waste bottle. This does not apply for etching epilayers.
There should be a bottle in the fumehood for HCl used to etch InP substrates.
Once the bottle is full, it should be brought to the basement of building 346 and a new one placed in the CR. For InP waste a clean and empty developer bottle can be used.
== GaAs substrate etching ==
When etching GaAs substrates, both 2” wafers and small pieces, you should collect the used chemicals in a waste bottle. This does not apply for etching epilayers.
There should be a bottle in the fumehood for citric acid: H2O2 or H2SO4 (10%):H2O2 used to etch GaAs substrates.
Once the bottle is full, it should be brought to the basement of building 346 and a new one placed in the CR. '''For the GaAs waste you should use empty H2O2 bottles (since they should have a special lid that avoid over pressure).'''


==HCl:H3PO4 etch==
==HCl:H3PO4 etch==


HCl(37%):H<sub>3</sub>PO<sub>4</sub>(85%) is a selective, anisotropic and slow etching of InP. Very slow rate in quarternaries. The etch rates depend on the orientation of the features and have not yet been calibrated at DTU Danchip.
HCl(37%):H<sub>3</sub>PO<sub>4</sub>(85%) is a selective, anisotropic and slow etching of InP. Very slow rate in InGaAsP. The etch rates depend on the orientation of the features and have not yet been calibrated at DTU Nanolab.


See rates below for InP, PQ(1.n) and InGaAs lattice-matched to InP. '''The acronym PQ(1.n) denotes a lattice-matched InGaAsP with a band gap corresponding to a wavelength of 1.n mm.'''  
See rates below for InP, PQ(1.n) and InGaAs lattice-matched to InP. '''The acronym PQ(1.n) denotes a lattice-matched InGaAsP on InP with a band gap corresponding to a wavelength of 1.n um.'''  


The temperature is 22 degC +/- 1 degC.
The temperature is 22 degC +/- 1 degC.


<!-- copyright issue rkc


{| border="1" style="text-align: center; width: 400px; height: 100px;"
{| border="1" style="text-align: center; width: 600px; height: 100px;"
! colspan="4" style="text-align: center;" style="background: #efefef;" | HCl(37%):H<sub>3</sub>PO<sub>4</sub>(85%) etch rates, nm/min
! colspan="5" style="text-align: center;" style="background: #efefef;" | HCl(37%):H<sub>3</sub>PO<sub>4</sub>(85%) etch rates, nm/min
|-
|-
! scope="row" width="20%" |Etchant
! scope="row" width="20%" |Etchant
Line 22: Line 50:
! width="20%" |PQ(1.1)
! width="20%" |PQ(1.1)
! width="20%" |InGaAs
! width="20%" |InGaAs
! width="20%" |Contributor
|-
|-
|1:4
|1:4
Line 27: Line 56:
|<2
|<2
|<1
|<1
|Before 2012 by Tine Greibe
|-
|1:0
|8700 +/- 500
|&nbsp;
|small
|2014-July by Luisa Ottaviano
|}
|}
<br>
-->


==H2SO4:H2O2:H2O etch==
==H2SO4:H2O2:H2O etch==


H<sub>2</sub>SO<sub>4</sub>(10%):H<sub>2</sub>O<sub>2</sub>(35%):H<sub>2</sub>O is a selective etch of InGaAsP with very low etch rate in InP. '''The acronym PQ(1.n) denotes a lattice-matched InGaAsP with a band gap corresponding to a wavelength of 1.n mm.'''  
H<sub>2</sub>SO<sub>4</sub>(10%):H<sub>2</sub>O<sub>2</sub>(30%):H<sub>2</sub>O is a selective etch of InGaAsP with very low etch rate in InP. '''The acronym PQ(1.n) denotes a lattice-matched InGaAsP on InP with a band gap corresponding to a wavelength of 1.n um.'''  


The etchrates have not yet been calibrated at DTU Danchip.
The etch rates have not yet been calibrated at DTU Nanolab.
The temperature is 22 degC +/- 1 degC.
The temperature is 22 degC +/- 1 degC.


<!-- copyright issue rkc


{| border="1" style="text-align: center; width: 500px; height: 100px;"
{| border="1" style="text-align: center; width: 800px; height: 100px;"
! colspan="6" style="text-align: center;" style="background: #efefef;" | H<sub>2</sub>SO<sub>4</sub>(10%):H<sub>2</sub>O<sub>2</sub>(35%):H<sub>2</sub>O etch rates, nm/min
! colspan="7" style="text-align: center;" style="background: #efefef;" | H<sub>2</sub>SO<sub>4</sub>(10%):H<sub>2</sub>O<sub>2</sub>(30%):H<sub>2</sub>O etch rates, nm/min
|-
|-
! scope="row" width="20%" |Etchant
! scope="row" width="15%" |Etchant
! width="20%" |InP
! width="10%" |InP
! width="20%" |PQ(1.1)
! width="15%" |PQ(1.1)
! width="20%" |PQ(1.3)
! width="15%" |PQ(1.3)
! width="20%" |PQ(1.5)
! width="15%" |PQ(1.5)
! width="20%" |InGaAs
! width="15%" |InGaAs
! width="100%" |Contributer
|-
|-
|1:1
|1:1:0 '''<sup>1</sup>'''
|<5
|<5
|<50
|<50
|230+/-70
|1000+/-500
|2700+/-1000
|Updated 2014-July by Luisa Ottaviano
|-
|10:8:71
|&nbsp;
|&nbsp;
|&nbsp;
|&nbsp;
|&nbsp;
|&nbsp;
|&nbsp;
|500
|Updated 2014-July by Luisa Ottaviano
|-
|10:8:171
|&nbsp;
|&nbsp;
|&nbsp;
|&nbsp;
|180+/-20
|Updated 2014-July by Luisa Ottaviano
|}
|}


==Concentrated H3PO4==
'''(1)''' The etch rates have not yet been calibrated at DTU Nanolab.
-->
<br>


Concentrated H<sub>2</sub>SO<sub>4</sub>(90%) is a selective etch of InP with a very low etch rate in InGaAsP.
==Concentrated H2SO4==


Concentrated H<sub>2</sub>SO<sub>4</sub>(98%) is used for deoxidation of InP with a very low etch rate in InGaAsP.


{| border="1" style="text-align: center; width: 500px; height: 100px;"
{| border="1" style="text-align: center; width: 500px; height: 100px;"
! colspan="6" style="text-align: center;" style="background: #efefef;" | H<sub>3</sub>PO<sub>4</sub>(90%) etch rates, nm/min
! colspan="6" style="text-align: center;" style="background: #efefef;" | H<sub>2</sub>SO<sub>4</sub>(98%) etch rates, nm/min
|-
|-
! scope="row" width="20%" |Etchant
! scope="row" width="20%" |Etchant
Line 70: Line 131:
! width="20%" |InGaAs
! width="20%" |InGaAs
|-
|-
|H<sub>2</sub>SO<sub>4</sub>(90%)  
|H<sub>2</sub>SO<sub>4</sub>(98%)  
|13
|13
|?
|?
Line 77: Line 138:
|&nbsp;
|&nbsp;
|}
|}
<BR>


==H3PO4:H2O2:H2O etch==
==H3PO4:H2O2:H2O etch==


H<sub>3</sub>PO<sub>4</sub>(85%):H<sub>2</sub>O<sub>2</sub>(35%):H<sub>2</sub>O is a GaAs/AlGaAs-etch which gives a better surface quality than H<sub>2</sub>SO<sub>4</sub>-based etches.
H<sub>3</sub>PO<sub>4</sub>(85%):H<sub>2</sub>O<sub>2</sub>(30%):H<sub>2</sub>O is a GaAs/AlGaAs-etch which gives a better surface quality than H<sub>2</sub>SO<sub>4</sub>-based etches.


<!-- copyright issue rkc


{| border="1" style="text-align: center; width: 500px; height: 100px;"
{| border="1" style="text-align: center; width: 500px; height: 100px;"
! colspan="4" style="text-align: center;" style="background: #efefef;" | H<sub>3</sub>PO<sub>4</sub>(85%):H<sub>2</sub>O<sub>2</sub>(35%):H<sub>2</sub>O etch rates, nm/min
! colspan="4" style="text-align: center;" style="background: #efefef;" | H<sub>3</sub>PO<sub>4</sub>(85%):H<sub>2</sub>O<sub>2</sub>(30%):H<sub>2</sub>O etch rates, nm/min
|-
|-
! scope="row" width="30%" |Etchant
! scope="row" width="30%" |Etchant
Line 104: Line 168:
|~600
|~600
|~600
|~600
|'''2,3'''
|'''2, 3'''
|}
|}


'''(1)''' Temperature of mixture is ~22 C (no heating during etch). data obtained using magnetic stirring with sample on flat basket. '''(2)''' Refrigerated H2O used during mixture of etch, and mixture kept at 17 C during etch. '''(3)''' 10:2:30 gives smoother etch than 10:2:60.
'''(1)''' Temperature of mixture is ~22 degC (no heating during etch). Data is obtained using magnetic stirring with sample on flat basket. '''(2)''' Refrigerated H2O used during mixture of etch, and mixture kept at 17 degC during etch. '''(3)''' 10:2:30 gives smoother etch than 10:2:60.


==BHF etch==
-->


BHF etches SiO<sub>2</sub> and removes native oxide on InGaAs. '''Do not use BHF unless you know the dangers involved with this chemical and always use 4H gloves!'''.
<br>


==BHF, HF etch==
BHF etches SiO<sub>2</sub> and partially removes native oxide on InGaAs and InP. '''Do not use BHF unless you know the dangers involved with this chemical and always use 4H gloves!'''.
<!-- copyright issue rkc


{| border="1" style="text-align: center; width: 500px; height: 100px;"
{| border="1" style="text-align: center; width: 500px; height: 100px;"
! colspan="4" style="text-align: center;" style="background: #efefef;" | BHF etch rates, nm/min
! colspan="5" style="text-align: center;" style="background: #efefef;" | BHF (12.5%), HF etch rates, nm/min
|-
|-
! scope="row" width="30%" |Etchant
! scope="row" width="15%" |Etchant
! width="20%" |SiO<sub>2</sub> '''<sup>1</sup>'''
! width="25%" |SiO<sub>2</sub>
! width="20%" |PECVD2 Si<sub>3</sub>N<sub>4</sub>
! width="20%" |PECVD2 Si<sub>3</sub>N<sub>4</sub>
! width="20%" |E-beam Ti '''<sup>2</sup>'''
! width="20%" |E-beam Ti '''<sup>1</sup>'''
! width="20%" |Al(x)GaAs, x>0.5, AlAs
|-
|-
|BHF 1:7
|BHF (12.5%)
|202
|283 '''<sup>2</sup>''', 175+/-25 '''<sup>3</sup>'''
|52
|88 '''<sup>4</sup>'''
 
|90-120
|90-120
|&nbsp;
|-
|HF:H<sub>2</sub>O
|&nbsp;
|&nbsp;
|&nbsp;
|>10000 '''<sup>5</sup>'''
|}
|}


'''(1)''' Process '''SiO2thi1''' in PECVD2. '''(2)''' Ti from Titest.prg on Physimeca. It seems there is no measurable etchig during first 10 seconds.
'''(1)''' Ti from Titest.prg on Physimeca. It seems there is no measurable etching during first 10 seconds.<br>
'''(2)''' Process '''SiO2ky2''' in PECVD2 (2014-July Luisa Ottaviamo @photonics ). <br>
'''(3)''' Process '''STANDARD''' in PECVD2 (2014-July Luisa Ottaviano @ photonics).<br>
'''(4)''' Process '''SINSTD''' in PECVD2 (2014-July Luisa Ottaviano @ photonics). <br>
'''(5)''' Appl. Phys. Lett. vol. 51, 2222 (1987).
<br>
<br>'''Note:''' neither Physimeca or PECVD2 is available anymore. Use the Temescal and the PECVD3/PECVD4 instead.
 
-->


==Citric Acid etch==
==Citric Acid etch==
Line 135: Line 219:
C<sub>6</sub>H<sub>8</sub>O<sub>7</sub>:H<sub>2</sub>O<sub>2</sub> is a selective etch of GaAs; does not etch Al<sub>x</sub>Ga<sub>{1-x}</sub>As if x > 0.45.
C<sub>6</sub>H<sub>8</sub>O<sub>7</sub>:H<sub>2</sub>O<sub>2</sub> is a selective etch of GaAs; does not etch Al<sub>x</sub>Ga<sub>{1-x}</sub>As if x > 0.45.


Solid C<sub>6</sub>H<sub>8</sub>O<sub>7</sub> is mixed 1:1 by weight with H<sub>2</sub>O using magnetic stirring. The solution C<sub>6</sub>H<sub>8</sub>O<sub>7</sub>:H<sub>2</sub>O is thereafter mixed 4:1 volume ratio with H<sub>2</sub>O<sub>2</sub>.
Solid C<sub>6</sub>H<sub>8</sub>O<sub>7</sub> is mixed 1:1 by weight with H<sub>2</sub>O (30%) using magnetic stirring. The solution C<sub>6</sub>H<sub>8</sub>O<sub>7</sub>:H<sub>2</sub>O is thereafter mixed 4:1 volume ratio with H<sub>2</sub>O<sub>2</sub>.
 
The above C<sub>6</sub>H<sub>8</sub>O<sub>7</sub>:H<sub>2</sub>O<sub>2</sub> solution has an etch-rate of ~360 nm/min in GaAs and < 0.5 nm/min in AlAs @ 25 degC.
 
==More info regarding etching of III-V materials==
 
More info on etching of III-V materials (not the DTU Nanolab wiki) can be found here:
 
https://wiki.nanofab.ucsb.edu/wiki/Wet_Etching_Recipes '''(at the UCSB Nanofab Wiki)'''
 
and


The above C<sub>6</sub>H<sub>8</sub>O<sub>7</sub>:H<sub>2</sub>O<sub>2</sub> solution has an etch-rate of ~360 nm/min in GaAs and < 0.5 nm/min in AlAs @ 25 C.
https://www.sciencedirect.com/science/article/pii/S0927796X00000279 '''(at the UCSB Nanofab Wiki)'''