Wet Chemical Etching
Safety
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Etchant materials are extremely corrosive.
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Wear eye goggles, face shield, nitrile gloves, vinyl lab apron, non-woven
material shoes.
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Add acid to diluent.
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Add stronger acids to weaker acids.
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Add oxidizer last.
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Material Selectivity |
Etchant |
GaAs |
InP |
InGaAs |
InGaAsP |
GaInP |
GaAsP |
AlGaP |
AlGaAs |
AlInP |
InAlAs |
InGaAlAs |
SiO2 |
HCL : H3PO4 |
S |
E |
S |
S |
E |
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E |
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H3PO4 : H2O2
: H2O |
E |
S |
E |
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S |
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H2SO4 : H2O2
: H2O |
E |
S |
E |
E |
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C6H8O7 : H2O2 |
CD |
S |
CD |
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CD |
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CD |
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HCL : HNO3 : H2O |
E |
E |
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E |
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E |
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HNO3 : H2SO4 : H2O |
E |
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E |
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HCL : H2O2 : H2O |
E |
E |
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E |
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HCL : H2O |
S |
E |
S |
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E |
CD |
CD |
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BHF : H2O |
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CD |
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E |
Legend |
Etches |
Selective/Stops |
Composition Dependent |
No Data |
E |
S |
CD |
|
Ga2O3 Etchants
References: (2 [sec. 4.3.2], 8, 98, 99).
Ga2O3 thickness typically ~<50 Å.
1:1 - HCL : H2O --- (10 sec.)
1:20 - H2SO4 : H2O --- (30 sec.)
1:40 - H3PO4 : H2O --- (20 sec.)
HCL : H3PO4
References: (4, 9, 10, 99).
Reaction rate limited.
InP etch rate with 1:1 ~2.5 µm/minute.
GaInP etch rate with 1:1 ~0.60 µm/minute.
H3PO4 : H2O2 : H2O
References: (13, 98, 99).
Reaction rate limited.
GaAs etch rate with 3:1:25 ~0.30 µm/minute.
InGaAs etch rate with 1:1:8 ~0.40 µm/minute.
InGaAs and InAlAs etch rates with 1:1:38 ~0.10 µm/minute.
H2SO4 : H2O2 : H2O
References: (1, 2, 3, 14).
Diffusion rate limited above ~33% H2SO4.
Reaction rate limited below ~ 33% H2SO4.
Etch rates proportional to Ga and As content.
InGaAsP etch rate with 1:1:10 ~0.10 µm/minute.
C6H8O7 : H2O2
References: (5, 6, 7, 16).
Reaction rate limited.
References (5, 16) prepares citric acid solution = 1 gram C6H8O7
(anhydrous) : 1 ml H2O. Various selective and non-selective
etchants are obtained by varying the volume ratio of citric acid to hydrogen
peroxide (after refs. 5, 16):
|
Etch Rate Å/min. |
C6H8O7 : H2O2 |
GaAs |
Al0.3Ga0.7As |
In0.2Ga0.8As |
In0.53Ga0.47As |
In0.52Al0.48As |
InP |
InAs |
Al0.5Ga0.5Sb |
GaAs0.85Sb0.15 |
GaSb |
1 : 2 |
60 |
27 |
346 |
1235 |
21 |
12 |
655 |
0 |
41 |
7 |
1 : 1 |
69 |
27 |
751 |
1116 |
22 |
11 |
826 |
0 |
47 |
6 |
2 : 1 |
85 |
24 |
1442 |
1438 |
26 |
9 |
n/a |
n/a |
n/a |
9 |
3 : 1 |
2169 |
24 |
2318 |
n/a |
n/a |
n/a |
n/a |
n/a |
n/a |
n/a |
4 : 1 |
2235 |
23 |
2777 |
n/a |
n/a |
n/a |
n/a |
n/a |
n/a |
n/a |
5 : 1 |
3140 |
27 |
2588 |
1433 |
44 |
5 |
895 |
0 |
52 |
9 |
7 : 1 |
2882 |
89 |
2231 |
1421 |
63 |
3 |
n/a |
n/a |
1523 |
n/a |
10 : 1 |
2513 |
1945 |
1219 |
1020 |
154 |
4 |
727 |
0 |
1284 |
7 |
15 : 1 |
1551 |
1082 |
882 |
1013 |
n/a |
n/a |
n/a |
n/a |
n/a |
n/a |
20 : 1 |
762 |
918 |
624 |
665 |
204 |
2 |
473 |
0 |
997 |
7 |
50 : 1 |
397 |
512 |
384 |
303 |
174 |
5 |
n/a |
n/a |
n/a |
n/a |
References (6 & 7) employ citric acid monohydrate which results
in different etch rates and selectivity thresholds than those in the table.
Reference (16) gives a conversion of 1 gram C6H8O7
(monohydrate) : 0.829 ml H2O, which gives results within 10%
of the table. Reference (7) reports AlGaAs etch rates to be a function
of Al composition with no etching occuring for AlxGa 1-xAs
(x > 0.7), and selective etching for AlxGa1-xAs /
AlyGa1-yAs (x<0.5, y>0.7) with C6H8O7
: H2O2 / BHF : H2O. Results of experiments
at LPS with 5:1 for GaAs over AlAs were similar to those in the table for
GaAs / AlGaAs.
HCL : HNO3 : H2O
References: (10, 11)
Varying ratios produce selective and non-selective etchants for AlInP/GaAs
and AlGaP/GaAs with etch rates dependent on material composition.
HNO3 : H2SO4 : H2O
References: (12)
Varying ratios produce selective and non-selective etchants for GaAsP
over GaAs.
HCL : H2O2 : H2O
References: (2, 12)
Varying ratios produce selective and non-selective etchants for GaAs
over GaAsP.
HCL : H2O
References: (10, 15).
AlInP etch rate with 1:2 ~0.45 µm/minute.
InAlAs etch rate with 3:1 ~0.65 µm/minute.
InGaAlAs (AlAs=0.34) etch rate with 3:1 ~0.11 µm/minute, and
(AlAs=0.20) = no observable etching.
BHF : H2O
References: (7)
SiO2 etch rate with BHF(6:1) and no H2O ~0.10
µm/minute.
Guidelines
for SiO2 / BHF Etching
AlGaAs etch rate in 1:25 BHF(7:1) : H2O varies with Al composition
from ~0 µm/minute (Al<0.70) to 1.0 µm/minute
(Al0.99).
References
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1.
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"Modern GaAs Processing Methods"
R.E. Williams, Chap. 5, 1990, Artech House.
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2.
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"InP HBTs: Growth, Processing, and Applications"
B. Jalali, S.J. Pearton, Chap. 3, 1995, Artech House.
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3.
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"Selective Etching of Gallium Arsenide Crystals in H2SO4-H2O2-H2O
System"
S. Iida, K. Ito, J. Electrochem. Soc., 118-5,
1971, p. 768.
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4.
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"Material-Selective Chemical Etching in the System InGaAsP/InP"
S.B. Phatuk, G. Kelner, J. Electrochem. Soc.,
126-2, 1979, p. 287.
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5.
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"Etch Rates and Selectivities of Citric Acid/Hydrogen Peroxide
on GaAs, AlGaAs, InGaAs, InAlAs, and InP"
G.C. DeSalvo, W.F. Tseng, J. Comas, J. Electrochem.
Soc., 139-3, 1992, p. 831.
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6.
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"Selective Etching of GaAs and AlGaAs with citric acid/hydrogen
peroxide solutions"
C. Juang, K.J. Kuhn, R.B. Darling, J. Vac. Sci. Technol
B, 8-5, 1990, p. 1122.
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7.
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"Selective etching of AlGaAs/GaAs structures using the solutions
of citric acid/H2O2 and de-ionized H2O/buffered oxide etch"
J. Kim, D.H. Lim, G.M. Yang, J. Vac. Sci. Technol.
B, 16-2, 1998, p. 558.
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8.
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"Wet Chemical Digital Etching of GaAs at Room Temperature"
G.C. DeSalvo, et al, J. Electrochem. Soc., 143-11,
1996, p. 3652.
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9.
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"Plasma and Wet Chemical Etching of InGaP"
J.R. Lothian, J.M. Kuo, F. Ren, S.J. Pearton, J. Elec.
Mat., 21-4, 1992, p. 441.
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10.
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"Wet Chemical Etching of AlInP"
J.W. Lee, S.J. Pearton, C.R. Abernathy, et al, J.
Electrochem. Soc., 142-6, 1995, p. L100.
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11.
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"Wet Chemical Etch Solutions for AlGaP"
J.W. Lee, C.J. Santana, C.R. Abernathy, S.J. Pearton,
J. Electrochem. Soc., 143-1, 1996, p. L1.
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12.
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"Selective and Non-Selective Wet Chemical Etching of GaAsP"
J. Hong, S.J. Pearton, Solid-State Electronics,
39-11, 1996, p. 1675.
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13.
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"Selective Chemical Etching of InP Over InAlAs"
Y. He, B.W. Liang, N.C. Tien, C.W. Tu, J. Electrochem.
Soc., 139-7, 1992, p. 2046.
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14.
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"A Slow Selective Etch for GaInAsP Grown on InP"
G.A. Ferrante, J.P. Donnelly, C.A. Armiento, J. Electrochem.
Soc., 130-5, 1983, p. 1222.
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15.
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"A Selective Etch for InAlAs over InGaAs and for Different
InGaAlAs Quaternaries"
N.J. Sauer, K.B. Chough, J. Electrochem. Soc.,
139-1, 1992, p. L10.
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16.
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"Citric Acid Etching of GaAsSb, AlGaSb, and InAs for Heterostructure
Device Fabrication"
G.C. Desalvo, R. Kaspi, C. Bozada, J. Electrochem.
Soc., 141-12, 1994, p. 3526.
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98.
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Oliver King.
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99.
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Fred Seiferth.
Notes
All etch rates approximate at room (~20-25oC) temperature.
Generalizations concerning etch rate limiting processes are for the
etchant solutions commonly used at LPS which contain relatively high proportions
of diluents.
Etch rates and etch profiles are usually influenced by the specific
crystal plane undergoing the etch process.
Etch rates can be influenced by dopants.