Journal of Crystal Growth 52 (1981) 219-226

O North-Holland Publishing Company

VAPOR G R O W T H OF D I A M O N D ON D I A M O N D AND OTHER SURFACES

B.V. S P I T S Y N , L.L. B O U I L O V and B.V. D E R J A G U I N

Institute of Physical Chemistry, Academy of Sciences of the USSR, Moscow, USSR

It is shown that diamond crystallization by chemical vapor deposition should preferably be carried out at reduced pressures.
Selective growth of diamond is ensured by introducing atomic hydrogen into the crystallization zone; this suppresses crystal-
lization of graphite. The growth rate of homoepitaxial diamond films reached 1 ~m/h at 1000°C; film properties were identical to
those of bulk crystals. The lattice parameter in boron-doped films (-0.I at.%) decreased by 0.0009 A; the film and substrate
parameters coincide at dopant concentrations of -1 at.%, and the semiconductor diamond film intergrows with the substrate
without stress. Diamond crystals up to several tens of microns in thickness were grown also on non-diamond substrates. At large
supersaturation, the crystal habit is octahedral and at low supersaturation, it is cubic. The linear growth rate is constant at the
early stages of crystal growth but then it diminishes to a level typical for the homoepitaxial growth of diamond films.

1. Introduction surface of the d i a m o n d seed crystal. T h e material

The unique combination of excellent
mechanical, physical, and chemical properties of
d i a m o n d has been the driving force for the
d e v e l o p m e n t of new and c h e a p e r m e t h o d s of
synthesis. Different fields of d i a m o n d ap-
plications both in research and industry can be
satisfied only by essentially different techniques
of crystallization. F o r instance, the u n i q u e elec-
trical and t h e r m a l properties of d i a m o n d , as a
h i g h - t e m p e r a t u r e s e m i c o n d u c t o r , can be fully
d e v e l o p e d only u n d e r the following strictly con-
trolled conditions of synthesis: layered structures
are grown, consisting of alternating dielectric and
semiconducting single crystalline d i a m o n d films,
with thickness of the o r d e r of o n e micron each.
Such conditions can be o b t a i n e d by m e a n s of
v a p o r growth techniques at r e d u c e d pressure,
that is in the region of metastability of d i a m o n d .
R e s e a r c h in this direction [1, 2] began almost at
the same time as the well-known w o r k on
d i a m o n d synthesis at ultrahigh pressures.
2. Physical and chemical crystallization
T h e simplest process of d i a m o n d crystalliza-
tion is the sublimation of graphite and sub-
sequent c o n d e n s a t i o n of the c a r b o n v a p o r on the
is transferred to the growing crystal due to the
t e m p e r a t u r e gradient b e t w e e n the source and the
substrate [3]. A l t h o u g h this process is, in prin-
ciple, possible, in practice it is inhibited by a
n u m b e r of factors:
(1) A c c o r d i n g to L E E D data [4], the d i a m o n d
surface retains the bulk structure up to tem-
peratures - 1 3 0 0 ° C (in vacuum). A t such tem-
peratures the equilibrium c a r b o n v a p o r pressure
o v e r the d i a m o n d phase is almost twice [3] that
o v e r graphite [5], and reaches - l × 10-13Torr.
A n acceptable growth rate (about 1/xm/h)
requires that the c a r b o n v a p o r pressure over
d i a m o n d phase exceed 10-6Torr. H e n c e , the
sublimation growth of d i a m o n d at such rates
requires supersaturation - - 1 0 7 which obviously
entails high defect density in the overgrowth. In
addition, the probability of nucleation and
growth of the graphite phase which is stable at
low pressures, will also be considerable at such
high supersaturations [6].
(2) T h e composition of c a r b o n v a p o r over
graphite shows a p r e d o m i n a n c e of C3-type
molecules [5] with multiple b o n d s between car-
bon atoms; this factor inhibits incorporation of
c a r b o n units into the d i a m o n d lattice.
(3) Finally, even single c a r b o n a t o m s in the
g r o u n d (non-excited) state are bivalent, so that
about 9 6 k c a l / g - a t o m has to be e x p e n d e d to

219
220 B. V. Spitsyn et al. / Vapor growth of diamond
transform them to the tetravalent state charac-
teristic of carbon atoms in the diamond struc-
ture.
A number of recently suggested techniques of
carbon condensation into a so-called "diamond-
like carbon" grown from excited carbon atoms
and ions on cold diamond and non-diamond
substrates [7-10] can be classified as physical
methods. Usually, dielectric layers grown by
these techniques contain only fragments of the
diamond structure, with grain size of the order of
1 0 ~ ; in some cases diamond crystallites with
sizes up to - 1 / z m were observed [9].
Chemical vapor deposition opens new pos-
sibilities for diamond crystallization in the region
of thermodynamic metastability. As indicated by
the published data, only this technique makes it
possible to achieve acceptable growth rates at
moderate supersaturations, and to grow perfect
homoepitaxial diamond films.
Let us compare the simplest processes of phy-
sical crystallization (PC) and chemical crystal-
lization (CC) of a solid A. In the case of PC,
consider a crystal in equilibrium with vapor of
the same composition:
A(gas) ~ A(solid).
In the case of CC, equilibrium sets on as a result
of a chemical reaction between crystal A(solid)
and vapor:
AB(gas) ~ A(solid) + B(gas).
We introduce supersaturation coefficients
defined as
Olphy s = pA/p°A, O~chern = PAR/pOAB,
where PA and PAB are actual partial pressures in
the condensation zone, and p o and p o are
equilibrium values. Let us assume that super-
saturation in the system is sufficiently high that
decrystallization may be neglected, but still too
low for homogeneous nucleation. Assuming now
the accommodation coefficient to be 1, we find
that t h e rate of physical crystallization is
Vphys= cl(PA - P°A) = Cl(aphys- 1)P ° (1)
(here and throughout the text ci are constants).
The rate of chemical crystallization depends both
on the supersaturation and on the energy of
activation E of decomposition of a molecule
AB(gas) at the substrate surface. Consequently,
in the approximation of direct impact the rate of
CC is
Vchem = c2(PAB-- P°m) e x p ( - E / R T )
= C~(achem-- 1)P ° e x p ( - E / R T ) . (2)
The dependence of p o and p O on crystallization
temperature T can be found by using the equa-
tions of chemical thermodynamics
P°A = C3 e x p ( - M R T ) ,
0 0
PAB/PB = Keq = exp(AG°T/RT),
where A is the heat of evaporation of the crystal
A(solid), AG ° is the change of the Gibbs free
energy in the chemical reaction, and Keq is the
equilibrium constant. By assuming
P ° ~ p ° ~- px,
we obtain
pO ~. p~ exp(A GO/ R T ) ,
where Px is the total pressure in the CC system.
Substitution of the expressions obtained for p o
and p o into eqs. (1) and (2) yields the super-
saturation necessary for achieving the desired
growth rate of the crystal:
O~phys ~ O p h y s C l l C ~ 1 e x p ( A / R T )
O%hem ~ UchemC21ex e x p ( - A G ° + E ) / R T .
If equal growth r a t e s ( U p h y s = Uchem) are realized at
the same temperature in the two methods, the
ratio of supersaturation is
~/ = O/phys/Ogchem
const. Pz exp[(AG ° - E + A )/RT]. (3)
This ratio is a relative measure of the advantage
of CC compared to PC. If y >> 1, the CC-grown
 B. V. Spitsyn et al. / Vapor growth of diamond
crystal will presumably be of greater perfection
than crystals grown by PC-methods at the same
rate and at the same substrate temperature, since
in this case O~chern"~ O~phys. For instance, hydrogen
reduction of tungsten fluoride at -850°C [11]
produced single-crystalline tungsten layers with
the theoretically predicted density. Physical
sublimation of tungsten cannot lead to similar
results. According to eq. (3), the advantages of
CC compared to PC are enhanced as the crystal-
lization temperature is lowered and the pressure
Px increased. However, this increases 0~chem , and
may cause a deterioration of the quality of the
deposits. The above analysis obviously suffers
from idealizations, since it neglects mass transfer
in the gas phase, diffusion in adsorption layers,
and possible concurrent reactions in the bulk and
on the crystal surface.
Growth rates and crystal perfection are very
different in different modifications of the chem-
ical crystallization techniques. For example, the
well-known method of growth on diamond seed
crystals by methane pyrolysis [2, 6, 12] is charac-
terized by a low linear growth rate and by an
unavoidable deposition of graphite. This makes
the method suitable only for increasing the mass
of highly dispersed diamond powders in a cyclic
process involving a periodically repeated remo-
val of non-diamond carbon from the surface of
fine powder diamond. High-perfection single-
crystalline layers with thickness of the order of
several microns can be grown only in a selective
process (suppressing the deposition of graphite)
which provides a substantially higher linear
growth rate. We have achieved this goal by using
a chemical transport reaction (CTR) for the
growth of diamond. Table 1 gives the main
Table 1
Synthesis of diamond by pyrolysis of CH4 and by the chemical transport reaction
techniques (CTR)
Process characteristics
Growth rate at 1000°C Ozm/h)
Epitaxial layer thickness (p,m)
Threshold temperature of epitaxial growth (°C)
Activation energy (kcal/mole)
Graphite deposition
Pressure in the gas phase (atm)
221
characteristics of this new process and of the
pyrolysis of methane.
CTR synthesis of diamond was carried out
from hydrocarbons in a closed system, by carbon
transfer from a graphite source to a diamond
substrate. The gas medium obtainable according
to the mode of chemical transport reaction con-
tains the following simplest hydrocarbons:
methane, ethane, ethylene, acetylene supplying
carbon to the diamond surface. Selectivity of the
process was achieved by introducing an increased
concentration of atomic hydrogen. The latter
interacts strongly with graphite but practically
does not affect diamond [13]. Different methods
are available for obtaining a superequilibrium
concentration of atomic hydrogen. The selective
etching effect with regard to graphite was nearly
the same when the thermal (several % H) and
the electric discharge (about 10% H) methods
were used for obtaining a superequilibrium con-
centration of atomic hydrogen. But it is neces-
sary to note that within the temperature range
between 800 and 1200°C, we obtain virgin
diamond, not graphitized at 1500°C in vacuum,
in contrast to the so-called diamond-like carbon.
Because of the multicomponent nature of the
system and the large number of reactions taking
place in the gas phase and on the surface of the
substrate (hydrogenation of hydrocarbons, recom-
bination of atomic hydrogen, and the crystal-
lization process itself), the absolute value of the
supersaturation could not be determined. The
growth rate depends on the character and tem-
perature of the substrate, on the partial pressures
of the components, and on the geometry of the
system. According to ref. [14], in the CTR mode
the supersaturation at the substrate increases
Pyrolysis of CI-I4 CTR
0.001 -1
0.002 5
-850 --750
60 25
Yes No
0.001-0.5 0.01-0.5
222 B. V. Spitsyn et al. / Vapor growth of diamond
when the crystallization t e m p e r a t u r e decreases
and the partial pressure of the c o m p o n e n t com-
prising the crystallized material increases. In the
synthesis techniques that we have chosen, the
supersaturation is a function of both the pressure
of hydrocarbons, and of the partial pressure of
atomic hydrogen. The latter changes the concen-
tration of the hydrocarbon complexes adsorbed on
the substrate, by interacting with hydrocarbons in
the gas phase and on the surface. Hence, the
atomic hydrogen not only maintains selectivity of
the process but also affects the growth rate, thus
having the role of an active participant in the
diamond crystallization.
3. Diamond growth on diamond surfaces
Substrate t e m p e r a t u r e is one of the factors
which determines the rate of the process and the
structure of the deposit. D i a m o n d layers grown
on single crystals at 600°C are polycrystalline
with grain size of 15 to 2 0 ~ [15]. However,
high-perfection single-crystalline layers were
obtained on the {110} face of natural diamond at
750°C; this is confirmed by electron diffraction
(fig. 1) which shows a well-pronounced system of
Fig. 1. Electron diffraction pattern (E= 65keV) of a
diamond film 0.8/~m thick, grown on {110} face of a natural
diamond crystal at a growth rate -0.4/.*m/hour.
Kikuchi lines. As the t e m p e r a t u r e is increased
further, the growth rate of homoepitaxial film
increases (activation energy of the order of
25kcal/mole) and reaches a m a x i m u m at
1000°C. Further increase in t e m p e r a t u r e results
in reduction of the growth rate and in deteriora-
tion of the structure of the diamond layers, so
that H E E D analysis reveals graphite inclusions.
Cathodoluminescence [17] and X-ray topo-
graphy [16] have d e m o n s t r a t e d that void-type
growth defects produce stresses in homoepitaxial
diamond films. As the crystallization tem-
perature is lowered from 1100 to 800°C, the
stress in the film increases by a factor of ap-
proximately three. When the stresses in the
substrate-film system exceed a certain threshold,
lattice discontinuities and microtwin lamellae are
formed in the film [18]. At the same time, E S R
studies show that the film contains broken C - C
bonds. Stresses produced during growth and high
rates of crystallization may result in deterioration
in the morphology of the diamond deposit (fig. 2)
and in a gradual transformation from a single-
crystalline film into a polycrystalline one. The
diamond layers were characterized (using SIMS)
by a comparatively high purity [19]; the impurity
content was found to be approximately the same
as in natural single crystals. One exception is
Fig. 2. Diamond layer ~4/xm thick, grown at a rate of
- 2 p.m/hour on {111}face of a natural crystal.
 B. V. Spitsyn et al. / Vapor growth of diamond
Table 2
Some properties of synthetic diamond
Property
Lattice constant (22°) (/~)
Carbon content (%)
Refractive index
Microhardness on (111) (kg/mm2)
Transmittancy in the UV range (nm)
Dielectric constant
Electrical resistivity (ohm cm)
hydrogen which has a concentration in homoe-
pitaxial films about twice that in natural
diamond. An increased hydrogen content in
CTR-grown diamond is caused by the active role
of atomic hydrogen in this process. Within the
experimental errors, the properties of the syn-
thetic and natural diamond are identical (see
table 2).
4. Semiconducting diamond
Introduction of gaseous boron compounds in
the process of diamond deposition made it pos-
sible to grow and investigate [19] single-crystal-
line semiconducting diamond films. As the
doping level is increased from -1017 to
~10Wcm -3, the activation energy of electrical
conduction falls from 0.37 to - 0 . 1 e V .
Measurements of thermo-emf and Hall effect
demonstrated that the semiconducting diamond
layers have p-type conductivity. As shown by
X-ray topography data, boron doping to a con-
centration - 0 . 1 a t % decreases the lattice
parameter of synthetic diamond by 0 . 0 0 0 9 ~
[16]. The lattice contraction and hole conduc-
tivity of diamond indicate that, at low doping
levels, boron atoms are mostly found in lattice
sites. The lattice parameter of the highly doped
(up to - 1 a t % boron) semiconducting diamond
is practically equal to that of the substrate. It
appears that in this case the film contraction due
to boron incorporation in lattice sites is com-
pensated by lattice expansion due to interstitial
boron atoms.
223
Synthetic diamond Naturaldiamond
3.5664± 0.0001 3.5668_+0.0001
100 100
2.38 ± 0.2 2.40
9500 - 400 8500-11000
~>225 />225
4-6 5.8
10Jz-1013 1013-1015
Boron is mostly incorporated into the {111}
faces and the incorporation on {100} faces is very
low. The electric conductivity of {100} diamond
films is lower by approximately a factor of 104
than that of films grown on {111} faces. Boron
differs in its electronic structure from the carbon
atom which it replaces, and the diamond lattice
near a dopant atom undergoes a distorition.
Also, boron has a valence equal to 3 and can be
incorporated more easily into a {111} face having
three-fold bonding. This, in the authors' opinion,
is one of the causes of a preferred incorporation
of boron during the growth of {111} diamond
faces.
5. Diamond growth on foreign surfaces
One of the reasons permitting the nucleation
of diamond on foreign substrates is the sup-
pression of the graphite deposition in the
presence of atomic hydrogen. A n o t h e r reason is
related to the weak effect of the substrate surface
forces on the nucleation under the conditions of
comparatively high supersaturation realized in
the C T R technique.
Diamond crystallization on foreign surfaces
was conducted under synthesis conditions typical
for homoepitaxial growth but poly- or single-
crystalline Cu, Si, W, or other substrates were
used instead of diamond seed crystals. Spon-
taneous nucleation of diamond crystals was
observed mostly on defects like scratches, grain
boundaries, dislocation outcrops etc.; this sup-
ports the assumption that nucleation takes place
on the substrate and not in the gas phase.
224 B. V. Spitsyn et al. / Vapor growth of diamond
The rate of nucleation (determined by the
number of diamond crystals formed on a speci-
men) varies from 103 t o 108 c m -2 h -1, depending
on the synthesis conditions, substrate material,
the method of preparation of the substrate (pol-
ishing, etching, annealing, etc.). The diamond
nucleation rate on carbide-forming substrates (Si,
Mo, W) is one to two orders of magnitude higher
than on substrates that do not form carbides
(Cu, Au); and it is several times lower on single-
crystalline substrates than on polycrystalline
substrates of the same material (after identical
preliminary treatment). The nucleation rate on
foreign substrates decreases as the substrate
coverage with diamond increases, and the num-
ber of nucleation centers and crystal size in-
crease.
Diamond crystals growing on substrates not
forming carbides usually have a well-defined
habit of regular half-polyhedra. By measuring
their linear dimensions in an optical microscope,
one can find the ratio vloo/Vm of growth rates in
the (100) and (111) directions; this ratio deter-
mines the crystal habit. Lowering of super-
saturation changes the habit from octahedral
(Vloo/VH1/>3) to cubic (Vloo/Vm ~<~/3/3), via in-
termediate cubo-octahedral forms. Fig. 3 shows
the ratio VloO/VH~as a function of supersaturation
which was varied only by the crystallization
temperature (maintaining all other parameters of
the CTR constant). Under the selected synthesis
conditions, octahedra grew at -800°C, and
V, oo Mill
1.7
>(
1.3
El.9
iDho T°E
Fig. 3. Crystal habit as a function of crystallization tem-
perature.
regular cubo-octahedra (Vloo/Vlll= X/3/2) at
1000°C. According to fig. 3, crystals with cubic
habit must grow at temperatures above the mel-
ting point of the copper substrate normally
employed. Therefore, the growth of such crystals
is facilitated at lower supersaturations, that is at
reduced concentrations of hydrocarbons.
Together with the single crystals, twins consis-
ting of two, five, or twenty single-crystalline units
joined along {111}, are also observed on the
substrate surface. Formation of such twins at the
very first stages of crystallization, and their
regular shape, indicates that these are nucleation
twins, and that the stable diamond nucleus on a
foreign substrate is formed from a large number
of carbon-containing complexes adsorbed on the
surface. The twinning probability is known to be
an increasing function of supersaturation [20]; a
considerable density of nucleation twins (up to
50% of the total number of crystals nucleated on
the substrate) indicates that the synthesis takes
place at a relatively high supersaturation.
Twins are also formed at later stages of crys-
tallization; from fig. 4a it can be seen that at least
part of the overgrowths on octahedral faces are
twins, which is proved by their mutual dis-
orientation. The growth twins were observed
both on {111} faces (fig. 4a) at Vloo/Vm< 0 . 9 and
on {100} faces (fig. 4b) at vloO/Vlll>0.9. Crystal
faces on which growth twins are formed usually
reveal one or several systems of concentric
macrosteps with twins in the center. Adjacent
faces of the same crystals not distorted by twin-
ning ({100} and {111} faces in figs. 4a and 4b,
respectively) are considerably smoother. The
appearance of growth twins is an obstacle to
growing diamond single crystals larger than
several tens of microns (at acceptable growth
rates).
It is interesting to compare the growth of
crystals nucleated on a foreign surface and of
diamond crystals intentionally placed on the sur-
face before the growth stage; the latter were
either fragments of natural single crystals, or
diamond crystals synthesized at ultrahigh pres-
sures. For such a comparison, we placed preli-
minarily oxidized (to remove foreign matter and
submicron diamond particles sticking to the main
grain) rounded-shape seed crystals on the surface
 B. V. Spitsyn et al. / Vapor growth of diamond 225

Fig. 4. Growth twinning on (a) {111}, and (b) {100}, faces.

of a polycrystalline copper specimen annealed in

hydrogen (fig. 5a). A f t e r a certain growth time
the specimens were extracted from the reactor,
p h o t o g r a p h e d in a scanning electron microscope,
and then returned to the reactor. A conducting
gold layer was not found necessary to obtain an
image when applying a scanning electron micro-
scope to photograph d i a m o n d crystals, having
sizes up to 50/,tin, that were grown on a conduc-
ting substrate.
Figs. 5b and 5c show the same area of the Fig. 5. Growth of diamond crystals on copper substrate: (a)
copper substrate as that in fig. 5a, after 15 area of substrate with two rounded-shape diamond seed
and 30 rain of growth. Crystals spontaneously crystals; (b) and (c) same area after 15 and 30 min of crystal-
nucleated on the substrate surface are seen to lization, respectively.
226 B. V. Spitsyn et al. / Vapor growth of diamond
grow with the same growth and faceting mode as
the diamond seed crystals. The crystal habit,
morphology, and growth rate become identical
for all types of diamond seed crystals (spon-
taneously nucleated, natural, and synthesized at
high pressures) after approximately 30min of
growth. The transient process is caused by the
irregular shape of the rounded crystals and by a
sharp increase in the number of crystallization
centers as a result of spontaneous nucleation.
After the crystals placed on the substrate achieve
a steady-state growth form, they differ from
spontaneously nucleated crystals only in a larger
size and in the absence of growth twins.
During the course of growing seed crystals on
a copper substrate, the authors have not noticed
any formation of twins on their surface during
about one hour. No further growth was carried
out because the surface of the copper substrates
was overgrown by spontaneously nucleated crys-
tals and because the linear growth rate has been
diminished on that account.
The linear growth rate of diamond crystals
spontaneously nucleated on the foreign surface is
constant during the initial stages of growth
(-5/.~m/h in the above example) but then falls as
the substrate coverage by diamond overgrowth
increases. After the surface is completely
covered with a polycrystalline layer, the linear
growth rate becomes nearly that characteristic of
the homoepitaxial diamond film under compar-
able synthesis conditions.
Acknowledgements
The authors are grateful to A.E. Aleksenko
and A.A. Botev for participation in the experi-
ments, to A.E. Gorodetsky for electron diffrac-
tion studies, and to Z.E. Sheshenina for SEM
photographs of the specimens.
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