Nagai Tilt XRD
Nagai Tilt XRD
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Deformation of the crystal lattice of layers of Gaxlnt_xAs (0.5 < x < 1.0) grown onto GaAs
substrates by a chemical vapor deposition process was investigated. For this study, Ga and In were
transported as chlorides with HCl and AsH) was the source of As. It was observed that the lattice
constant along the direction of the film thickness was larger than that along the surface. This fact
indicates that the crystal lattice of GaxIn t _ xAs is compressed along the substrate surface as a result
of lattice mismatch. The influence of both the composition of the epitaxial layers and the crystal
plane of the substrate surface on the degree of this deformation was investigated. It was also found
that the epitaxial orientation grew inclined to the substrate crystal when the crystal surface of the
substrate was pOO j or {II OJ.
II. EXPERIMENT
GaxIn1-xAs crystals were grown on GaAs substrates in
the temperature range 700-750°C. The apparatus used
for the growth was the same as that used for the vapor
growth of GaAs by a Ga-HCI-AsHs-H2 system, where
Ga-In alloys were used instead of Ga. The examined
crystalline orientation of the GaAs substrate were {100}
and {lll}. The cutting accuracy of the substrate surface
was made within 1°. The substrate surface was treated
by two methods. One method is a chemical etching by a
4 H2S04 : 1 H20: 1 Il20 etching solution at 80-90 °C, and
the other method is a mechanochemical polish. The
thickness of the substrates was in the range 2-5 mm,
and the epitaxial layer was in the range 5-10 Mm. In
this case the bending of the system 4 ,6 can be neglected. FIG. 1. Relation between the epitaxial and the substrate crys-
Generally, deposited crystals were undoped n type with tal lattice.
3789 Journal of Applied Physics, Vol. 45, No.9, September 1974 Copyright © 1974 American Institute of Physics 3789
3790 Haruo Nagai: Structure of vapor-deposited Gax In1_xAs 3790
~~2
090 0·80 070 0·60 050
(1) 0,=9,- 92 30
_ ~ Bragg
~=~==~r:J..:i~=d1 an~:
(2) O2=91- 92
two planes are inclined
Bragg angle 9, (1) 0;=(9,-92) + ~
..
::. Oe-Os
.~ as
.~
FIG. 2. Principle of the measurement of the angle between
the two crystal plane.
1·0 2·0 3·0 4·0
ideal misfit factor (%)
III. RESULTS
FIG. 4. Relief of the lattice mismatch by the deformation vs
A. Deformation of the crystal lattice mismatch factor.
1.0010
--...
{S11} diffraction
com
substrate (100)
0·9 0·8 0·7 0·6 0·5 0·4 FIG. 5. Reflection x-ray topographs of a {IOO} sample. Epi-
X (Ga x ln _ As) taxial layer is GaO.88InO.12As; thickness, 9 j,I m. Substrate
1x thickness, 5 mm. The discrimination between the (110) and
(IIO) axes was done by the method of etching in the
FIG. 3. Effect of the composition of the epitaxial layers on Cr03-HF-H20 system (Ref. 8). In this sample, the angle be-
the deformation of the epitaxial crystal lattice. The composi- tween the two {100} planes of the epitaxial layer and the sub-
tion was determined from the lattice constant. strate is 205".
TABLE 1. Inclination, deformation, and lattice constants TABLE II. Inclination of the epitaxial layers on different sub-
of the epitaxial layers on some different substrate surfaces. strate surfaces. [The composition of the epitaxial layer was
[The composition of the epitaxial layer was estimated to be estimated to be Gao.SsInO.12As from the lattice constant on sur-
Gao.SsInO.12As from the lattice constant on substrate surface (1). face (1). The thickness of the substrate was 2 mm, and that
The thickness of the substrate was about 4mm, and that of the of the epitaxial layer was 7 It m].
epitaxial layer was 7 It m on surface (1) J. 80 a
Substrate surface
Substrate surface 80 a d 100• t
b
d100•s !fullw. (sec)
(sec) (A) (A) d 100•s
along (110) , 55
(1) {I00}±1' 20 5.7132 5.6995 1.0024 along (110), 0
(2) 4.5 0 inclined along 540 5.7076 5.6962 1.0020 (2) 1. 0 inclined along {n 0)
0
along (11 0), 0
(110) from the surface from the surface of (1) along (110), 0
of (1)
(3) 1. 0 0 inclined along (110) along (110), 0
(3) 8. 8 0 inclined along 1100 5.7036 5.6962 1. 0013 from the surface of (1) along (110), 195
(110) from the surface
of (1) "Numbers following the directions are angles between the {IOO}
planes of the epitaxial and substrate crystaL
aAngles between the {100} planes of the epitaxial and substrate
crystal along the direction (11 0).
bd 100 •t and d 100 •s denote the lattice constant of the boo} along
the direction of the thickness and the direction of the surface, In the region x> 0.8, the degree of deformation in-
respectively. The calculation of the lattice constants was creases with the indium content, but in the region
performed assuming that the d 100 of GaAs that was used as the x < O. 8, it decreases with the indium content. When the
substrate was 5.6532 A. Measurement was made at 26 'C. values of lattice constant difference are small enough,
the mismatch is thought to be relieved only by the
5. The epitaxial layer is divided into two regions which elastic deformation of the crystal lattice of the epitaxial
have different orientatio~ of the {lOO} planes. The layer. When the mismatch reaches the limiting values,
boundary lies along the (110). Two regions divided by
one boundary are symmetric with respect to the inclina-
tion of the {IOO} plane. When the substrate surface was
treated by a mechanochemical polish, boundaries like
those of Fig. 5 were not seen, but the {lOO} planes of
Substrate surface 60
(sec) a
\-0,.,
~
(1) {Inho. 2° o '" ~(Olll-'"
(2) 3.0° inclined along (211) 187
from the surface of (1)
(3) 5.0° inclined along (211) 238
from the surface of (1)
FIG. 9. (a) and (b) Generation of the boundary line on the con-
cave substrate surface. (c) Epitaxial layer is GaO.97InO.osAs;
thickness, 16 p. m. The radius of curvature of the substrate
surface is 2 mm. (d) Epitaxial layer is GaO.96InO.04As; thick-
ness, 24 p. m. The radius of curvature of the substrate sur-
FIG. 7. Stacking-fault shadows on a {IOO} sample. face is 3mm.
experimentally.
substrate(100)j I I :mean value of step
The boundary on the convex surface can be observed +length
only by the x-ray topograph. No boundary exists on the epitaxial e/.. --,;-T----·n
surface of the epitaxial layer. But when the substrate layer(100)--,
surface is concave, the boundary appears on the \ ---4
epitaxial layer surface and can be observed by optical .-
f--
microscope. The substrate surface was prepared to
have a grooved configuration as shown in Fig. 9(a). The
two directions of the steps advance downwards to meet
with each other [Fig. 9(b)]' and a clear boundary line is
formed at the center, as shown in Fig. 9 (c). When the
epitaxial layer is grown on the spherical convex surface,
it is known that the facets are formed on the low-index
planes. 12 In this Ga"In1_~s-on-GaAs system, {lOO} fac- tan e/.. =A~
ets were found on the convex spherical substrate sur-
face. But when the substrate surface was a concave
FIG. 11. Model of the {100} interface between GaAs and
sphere, formation of the facets was not observed, and G~Inl-xAs. To simplify the condition, the lattice mismatch
the generation of the boundary line as shown in Fig. 9(d) in the horizontal direction is neglected in this figure. Actually,
was characteristic. This boundary line was found to when the step length 1 is large enough compared to the lattice
consist of an array of grooves by the optical interfer- constant of the epitaxial crystal, this condition will be satis-
ence method, and this seems similar to the grooves fied virtually by the effect of misfit dislocations and lattice
deformation. This model can explain the fact that the inclina-
which appears at the grain boundary when heated for a tion becomes small with the decrease of the lattice mismatch
long time. 13 and the inclination of the substrate surface from {lOO}.
steps, mismatch of the lattice constant may cause in- tration of a certain impurity may cause the difference
clination of the epitaxial layer as shown in this figure. of lattice constant, and it is known that the impurity con-
The mean value of the step length and the lattice mis- centration depends on the orientation16 of the substrate
match are the factors that decide the inclination. The surface even though the epitaxial layers are formed at
values of the inclination of {100} planes estimated from the same condition. Also, the change of the composition
this model lie near the values (15-250") obtained from can be a cause of lattice constant change in these terna-
the experiment. The reason why this phenomenon occurs ry compounds Therefore, the real cause of the change
0
only in the (110) and not in (110) is not explained by this of the lattice constant shown in Table I is not know yet.
model. This anisotropy between the (110) and (flO) di- Research is in progress concerning this point.
rections may be related to that observed in the bending 6
and misfit dislocations 14 of this heteroepitaxial system. V. CONCLUSIONS
When the inclination of the substrate surface from {100}
(0 In the Ga)n1_xAs-on-GaAs heteroepitaxial system,
becomes large [Fig. 10(c)], the mean length of the step
the crystal lattice of the epitaxial layer is deformed be-
becomes small. If this value is smaller than the dis-
cause of the lattice mismatch.
tance between the misfit dislocations which is expected
from the misfit factor, the lattice mismatch will not be (Ii) Besides the lattice deformation, the inclined
relieved sufficiently on each step. In this case, the sub- growth of the epitaxial layer was observed. (iii) The
grain boundarylike structure 15 is thought to be stable at crystal orientation of the substrate surface strongly af-
the interface. This will result in the more downward fects the phenomena mentioned above.
slope of the epitaxial layer as shown in Fig. 10(c). The
inclination of the substrate surface along (flO) or other ACKNOWLEDGMENTS
directions does not affect this phenomenon when it is
The author wishes to thank Dr. Y. Mizushima for
small (within about 1°), but the effect appears at a large
helpful discussions and suggestions. The author also
inclination angle. The same relation as in Fig. 10(c) is
wishes to thank T. Hattanda for his useful discussions.
observed in this case.
As has already been mentioned, tilting of the epitaxial
layer on {111} substrate was not initially observed. lC. J. Nuese and R. E. Enstrom, IEEE Trans. Electron
When the inclination of the substrate surface from {111} Devices ED-19, 1068 (1972).
is small (within about 1°), the epitaxial layer grows par- 2B. F. Williams, Appl. Phys. Lett. 14, 273 (1969).