Microwave microscopy of diamond semiconductor structures

A. N. Reznik, S. A. Korolyov, and M. N. Drozdov

Citation: Journal of Applied Physics 121, 164503 (2017); doi: 10.1063/1.4982676

View online: http://dx.doi.org/10.1063/1.4982676
View Table of Contents: http://aip.scitation.org/toc/jap/121/16
Published by the American Institute of Physics
 JOURNAL OF APPLIED PHYSICS 121, 164503 (2017)

Microwave microscopy of diamond semiconductor structures

A. N. Reznik,a) S. A. Korolyov, and M. N. Drozdov
Institute for Physics of Microstructures of the Russian Academy of Sciences, GSP-105,
Nizhny Novgorod 603950, Russia
(Received 16 February 2017; accepted 16 April 2017; published online 28 April 2017)
A scanning near-field microwave microscope (SNMM) was used to study resistance Rsh of a boron
delta-doped epilayer of diamond grown on a high pressure and high temperature substrate.
Measurements were performed with an 1.4 GHz working frequency and an 85 lm space
resolution microscope on samples with a lateral dimension of 3  3 mm2. Some substrates featured
a crystalline structure defect over which the epilayer resistance Rsh was seen to increase by more
than an order of 1 mm linear dimensions of the high-ohmic region. The SNMM measurement
data revealed some substrates to have nonuniform conductivity, i.e., a high-ohmic area in the cen-
tral part surrounded by a conducting edge region. In the latter case, the SNMM method allowed
determining a surface distribution of epilayer resistance Rsh, undistorted by the shunting influence
of the substrate. The reliability of the SNMM results is confirmed by the local four-probe resistance
measurements. At the same time, the alternative methods such as the non-local van der Pauw
method and secondary ion mass spectroscopy failed to detect the nonuniformity of the structure
conducting properties, established by SNMM. The obtained values for a hole concentration of
Np  1.7  1020 cm3 and a mobility of lH  15 cm2/(V s) are assumed to possibly pertain to the
diamond delta-layer. Published by AIP Publishing. [http://dx.doi.org/10.1063/1.4982676]

INTRODUCTION material. In the past 15–20 years, considerable success has

Present-day manufacturing technologies for devices and
elements of semiconductor micro- and nanoelectronics
involve characterization of samples in a variety of methods
and techniques. Among the most widely used ones are sec-
ondary ion mass spectroscopy (SIMS), capacitance versus
voltage C(V) measurements, Hall effects combined with four
probe resistivity measurements (commonly referred to as
the van der Pauw (VDP) method), optical ellipsometry, elec-
tron microscopy, infrared Fourier spectroscopy, probe
microscopy, X-ray structural analysis, and many others.
Simultaneous application of several probing techniques
allows one to get more information on structures in question.
Moreover, to upgrade the data reliability, it is useful to
employ tools that will ensure the determination of similar
parameters (for example, conducting or structural properties)
through independent measurements. In this connection of
great potential value are non-traditional methods that are
currently under development and testing. Of these, a very
promising technique is scanning near-field microwave
microscopy (SNMM).1–3 This method is characterized by a
high resolving power that exceeds the working wavelength
by many orders of magnitude. Modern microscopes in the
centimeter and decimeter wave range are capable of nanome-
ter resolution4–7 down to the atomic scale.8 Yet, a great
amount of research so far has been done based on medium
resolution (1–103 lm) devices.9–20 The important advantages
of SNMM rest on its capability for non-invasive nondestruc-
tive probing of objects not only on the surface but also in
depth. Another essential characteristic is the high sensitivity
of the microscope to the conducting properties of the
a)
Electronic mail: reznik@ipm.sci-nnov.ru
been achieved in quantitative SNMM diagnostics,9–11,20–25
making it possible to demonstrate the characterization poten-
tialities for semiconductors of yet a fairly simple structure—
bulk homogeneous or thin film ones.6,16,20,24,26 These
achievements give reason to believe that SNMM can find
wider applications in semiconductor technologies.
The key direction in the SNMM development over the
recent years has been towards achieving extremely high
(nanometer and subnanometer) spatial resolution, being
called for by the corresponding size of today’s electronic
components. It seems that there is an appropriate area of
application for medium-resolution SNMM as well, in particu-
lar, in working-out manufacturing technologies for new semi-
conductor materials. One promising material under active
investigation is semiconductor diamond.27 It is expected that
the predicted outstanding properties of diamond (large carrier
mobility, high breakdown voltage, and exceptional thermal
conductivity) will help improve the characteristics of semi-
conductor devices for high power and high frequency elec-
tronics. The main problems of semiconductor diamond
fabrication technology now include producing large-size
(>25 mm) single crystal diamond substrates, attaining high
values of free-carrier concentration (>5  1020 cm3) and
mobility (>103 cm2/(V s)), forming ultra-thin conducting
layers (<2 nm) by delta-doping, and realizing surface-
homogeneous characteristics of structures. The current
single-crystal diamond substrates are not more than 15 mm in
size. Due to the high cost of the substrates, studies are usually
conducted on samples of much smaller lateral dimensions
(the standard size is 3  3 mm2), which is quite an obstacle
for microwave diagnostics. Of the widest use are the sub-
strates grown by the temperature gradient method at high

0021-8979/2017/121(16)/164503/7/$30.00 121, 164503-1 Published by AIP Publishing.

164503-2 Reznik, Korolyov, and Drozdov
pressure and high temperature (HPHT).28,29 The HPHT sub-
strates, depending on the growth parameters, differ in their
crystalline quality and impurity content; they may have
growth sectors30 and other structural defects. Substrate
defects reveal about the structural and electrical properties of
epilayers that grow on them.31–33 Therefore, epitaxial growth
has to be controlled by local measurements. In this paper, we
show that a medium-resolution SNMM can serve as an effec-
tive tool for quantitative diagnostics of such structures.
SAMPLES AND METHODS
Diamond structures were grown on [100]-oriented
HPHT substrates with a lateral size of 3  3 mm2. We stud-
ied samples with boron p-doped delta-layers of 2–4 nm
thickness. The delta-doping of diamond proceeded during
epitaxial growth in a microwave plasma-enhanced chemical
vapor deposition (MPCVD) reactor with a rapid gas switch-
ing system.34 A typical thickness of the epilayers was
100 nm, although some samples had a 10–20 nm epilayer.
Diborane (B2H6 gas) was used as a source of boron.
Along with the SNMM, we also used the standard techni-
ques for characterization of semiconductor structures, such as
the SIMS method and VDP method. The SIMS method
was used for measuring a depth profile of boron atom concen-
tration NB(z) on a TOF.SIMS-5 setup. A series of test
structures—diamond layers implanted with 50 keV boronions
11
B in a varying dose—were fabricated for boron sensitivity
calibration. The VDP method35,36 yields hole concentration
Np and mobility lH within the epitaxial film-substrate system.
In this study, we used two geometries of VDP measurements,
specifically, the sample geometry (VDP-S) and the local
lamella-type geometry (VDP-L). For VDP-S measurements,
four ohmic contacts were formed in the corners of a test sam-
ple. In the VDP-L technique, five lamellar specimens were
shaped on a sample surface as electrically isolated Hall
crosses, i.e., outside the crosses, the epilayer was removed.
Each cross had four ohmic contacts formed in its corners (see
the inset in Fig. 5(a)). The overall size of a cross was
0.45  0.45 mm2, but the characterization target was a
0.15  0.15 mm2 area in the center of the cross. The arrange-
ment of crosses on a sample surface is shown in the insets in
Figs. 3(b), 5(a), and 5(b). Unlike the SNMM, the VDP-L
method involves several technological operations to be per-
formed during specimen fabrication, and the epitaxial film
has to be etched off almost completely. Also, note that VDP-
S measurements caused the destruction of the doped film in
the region where conducting contacts were formed with linear
dimensions of 200–300 lm. The same is true for SIMS
measurements whose by-effect on a sample is the formation
of a 100 lm diameter crater on its surface.
Our microwave microscope design is described in Ref.
20, where we also provide detailed information on the tech-
nique for determining resistance Rsh of a semiconductor film
on a dielectric substrate. The microscope is essentially a
1.4 GHz coaxial k/2 resonator with a probe in the form of a
sharpened tip, connected to the end of the resonator central
conductor. The informative parameters used to determine the
value of Rsh are a shift of resonance frequency f and a
J. Appl. Phys. 121, 164503 (2017)
change in the Q-factor when the probe comes in contact with
the sample. Resistance Rsh is calculated within the model of
an SNMM probe proposed in Ref. 20, which is basically a
monopole antenna. The fitting parameters for the model are
sought using a series of calibration etalons—dielectric quartz
(EQ), sapphire (ES), and conductive silicon plates varying in
a doping degree. For the studied diamond structures, it was
enough to use the two highest-resistance Si plates with resis-
tivity q ¼ 6000 and 52 X cm (etalons E0 and E1). The plates’
thickness was 0.4–0.7 mm. The microscope resolution power
depends on diameter dt of the probe tip end; according to the
micrography data, dt  40 lm. The actual resolution was
found from measurements of the parameters f and Q by scan-
ning a sample surface on which the metal and dielectric
regions were divided by a sharp line. The obtained value for
resolution d  85 lm proved to be poorer than expected from
dt measurements. In a study of diamond samples, the probe
tip was scanned over the sample surface {x, y} along the
axis [ (at y ¼ const) with a step D[  d. In every point of
the surface, the tip was brought in a “soft” contact with the
sample and then moved off the surface to a fixed height
Dz ¼ 0.3 lm, as described in Ref. 20. We measured the
microscope resonance curve (frequency dependence of reso-
nator reflectivity), upon which the probe was withdrawn to a
certain height z, moved one step D[ along the surface,
and the positioning/measuring procedure was repeated.
According to the test measurement data from Ref. 20 and
some additional studies, the error of Rsh measurements with
our coaxial SNMM does not exceed 50% at Rsh > 1 kX/sq.
Unlike in Ref. 20, we used the method developed therein
to determine resistance Rsh of the epilayer on a conducting
substrate and to measure resistivity q of the substrate itself.
The generalization of the method20 to these situations does not
cause any difficulties. It is suitable for testing planar structures
of any complexity, with one parameter to be determined Rsh or
q. The complex permittivity and thickness of all other layers in
the structure must be known. The SNMM model underlying
this technique allows the calculation of informative parameters
f and Q (i.e., a solution of the direct problem) for a structure
with any finite number of layers. To determine the single
unknown parameter of the structure (solution of the inverse
problem), we have designed a special computer algorithm,
enabling the partial automation of the measurement technique.
It is obvious that our approach assumes homogeneity of the
test structure on scale d, i.e., the characteristic scale of lateral
inhomogeneity of parameters Rsh and q must be larger than d.
As a first example of SNMM measurements, Fig. 1 repre-
sents dependencies of resonance frequency f and the Q factor
on coordinate x along scan lines 1–3 for sample De1. It is a
structure with an epilayer of a thickness of 80 nm including
five delta-layers varying in a peak concentration of boron
atoms. A SIMS depth profile of concentration NB(z) is shown
in Fig. 4(a). Profiles f(x) and Q(x) in Figs. 1(a) and 1(b),
respectively, characterize the inhomogeneity of structure De1.
Higher values for f and Q correlate with higher resistance val-
ues. The inset in Fig. 1(a) (and insets in Figs. 3(a), 3(b), and
5(a)) shows the high-ohmic region schematically designated
by dark ovals based on the SNMM scan data. The experimen-
tal data in Fig. 1(c) are presented in variables n and g, where
164503-3 Reznik, Korolyov, and Drozdov J. Appl. Phys. 121, 164503 (2017)

we can quickly estimate the lateral inhomogeneity of the sam-

ple under investigation. In particular, our experience in
SNMM measurements prior to the Rsh calculation allows us to
assert that sample De1 at points A1 and A3 differs in the resis-
tance value by about an order of magnitude. Besides, in the
low-ohmic region of the epilayer (vicinity of point A3), we
have Rsh > 10 kX/sq. Point Ds0 in Fig. 1(c) is the measure-
ment taken on a dielectric substrate. The location of this point
is determined by the real part of the diamond permittivity e:
e0 ¼ Re(e) ¼ 5.7 (for quartz, sapphire, and undoped silicon,
e0 ¼ 4.5, 10, and 11.7, respectively).
Diamond substrates often contain macroscopic defects of
a crystal structure. Some examples are substrates Ds1 and Ds2
whose 3D surface image is shown in Fig. 2. In contrast to
structures De1, De2, and De3 with an epilayer, we marked the
bare diamond substrates for corresponding samples as Ds1,
Ds2, and Ds3. The substrate images were taken with an
Optical Surface Profiler Zygo NewView 7300. Prior to imag-
ing, the surface had been treated by the H2/O2 plasma. In
Fig. 2, one can see the defective areas of 0.5–1 mm on the
substrates. The observed high resistance inhomogeneity in the
epilayer of sample De1 (see inset in Fig. 1(a)) is, in all proba-
bility, related to the structural defect on the substrate Ds1 sur-
face. The image of the latter in Fig. 2(a) coincides with the
high-ohmic region in the epilayer as measured by SNMM.

RESULTS AND DISCUSSION

Based on the SNMM studies, it has been established that
many of the diamond substrates have a laterally inhomoge-
neous conductivity. Application of the method20 to a bulk

FIG. 1. (a) Resonance frequency f and (b) Q-factor obtained by SNMM

scanning of sample De1 along lines 1–3. (c) Parameters f and Q in normal-
ized variables n and g. A1–A3 are the values for n and g in points on the sur-
face of sample De1, marked in (a) and (b). The line is the calibration curve
gc(n), calculated from measurements on etalons EQ, ES, E0, and E1. Point
Ds0 is the measurement on the dielectric diamond substrate. The inset in (a)
shows scanning lines 1–3 and the approximate location of the high-ohmic
region (dark ovals).

n ¼ (fEQ  f)/fEQ, g ¼ 0.5(1/Q  1/QEQ) are the normalized

resonance frequency and inverse value of the Q-factor; fEQ
and QEQ are parameters f and Q from a contact of the probe
with etalon EQ. The values A1–A3 in Fig. 1(c) correspond to
the three characteristic points on sample De1, indicated in
Figs. 1(a) and 1(b). The calibration curve gc(n) is plotted from
measurements on etalons EQ, ES, E0, and E1. The data in FIG. 2. Surface image of substrates (a) Ds1 and (b) Ds2. 1–3—SNMM scan
Fig. 1(c) provide the basis for realizing a method20 of deter- lines and ovals—the high-ohmic region. The arrow indicates the defect
mining resistance Rsh. Moreover, based on this information, location.
164503-4 Reznik, Korolyov, and Drozdov
sample such as a substrate, as mentioned above, yields resis-
tivity q. Figures 3(a) and 3(b) give the q profiles of substrates
Ds2 and Ds3. The nonuniform distributions of q(x,y) in Fig.
3—a high-ohmic region with q 10 kX cm in the central
part, with resistance decreasing towards the edges down to
q  0.1–1 kX cm—are quite typical for substrates under study.
The high-ohmic area on substrate Ds2 roughly corresponds to
the location of a defect, as shown in Fig. 2(b), whereas no
macro-defects were observed for Ds3. It should be noted that
our VDP-S measurements also revealed appreciable conduc-
tivity in a number of substrates. For example, the conductivity
of substrate Ds2, obtained by the VDP-S technique, was
q ¼ 0.8 kX cm. A comparison of this value with the SNMM
data in Fig. 3(a) clearly shows that such a value of q is charac-
teristic only of a substrate edge region. This conclusion is
fairly reasonable for objects with inhomogeneous conductivity
since by nonlocal VDP-S measurements, a direct current is
concentrated in low-resistance areas, which in our case corre-
sponds to the near-edge region of substrate Ds2. In contrast,
local SNMM measurements give a distribution q(x,y) in the
surface plane of a test sample.
The developed technique allowed us to obtain scan pro-
files of resistance Rsh of an epilayer that is grown, in particu-
lar, on an inhomogeneously conducting substrate. The
distribution q(x,y) of the substrate was first measured by the
FIG. 3. Resistivity profiles for substrates (a) Ds2 and (b) Ds3, scanned along
lines 1–3. The insets show scanning lines 1–3 and the approximate location
of the high-ohmic regions (dark ovals). The inset in (b) also shows the posi-
tion of Hall crosses.
J. Appl. Phys. 121, 164503 (2017)
SNMM method (for Ds2 and Ds3; see Fig. 3). After the
growth of the delta-doped epilayer, the film-substrate system
was scanned by SNMM approximately along the same lines.
The effect of the substrate conductivity was taken into
account in calculations of the epilayer resistance Rsh by the
method described in Ref. 20. Figure 5 shows the Rsh profiles
of the epitaxial film for samples De2 and De3. Scan lines 1
and 3 on sample De3 are interrupted due to the ohmic con-
tacts that had been formed in the corners of the structure for
VDP-S measurements. SIMS depth profiles of boron concen-
tration NB(z) in samples De2 and De3 are shown in Figs.
4(b) and 4(c), respectively.
The effect of substrate conductivity is the strongest on
SNMM measurements of structures with a high-ohmic epi-
layer, such as in sample De3 (see Fig. 5(b)). The average
over-all-points’ value of epilayer resistance is Rsh ¼ 250 kX/
FIG. 4. Depth profiles of boron atom concentration NB(z) for samples (a)
De1, (b) De2, and (c) De3. The inset in (b) shows points 1–3 on the surface
of sample De2, at which we obtained profiles NB(z).
164503-5 Reznik, Korolyov, and Drozdov
sq, and root-mean-square deviation rR ¼ 100 kX/sq. Based
on the measured profiles f(x) and Q(x), one could expect a
much higher inhomogeneity of the epilayer. The correspond-
ing effect was found to be related to the inhomogeneous con-
ductivity of the substrate, given a lower resistance of the
sample edge area. Indeed, a substrate with a thickness of
0.3 mm and resistivity q ¼ 0.2–11 kX cm (see Fig. 3(b)) has
a dc resistance of 7–370 kX/sq. Unlike the dc case, an ac
field does not penetrate the entire thickness of the substrate.
The depth of a microwave field penetration is determined by
a probe aperture size dt, and by our estimation, it is about
100 lm. So, the effective shunting resistance of a substrate,
arising from SNMM measurements of sample De3, proves to
be 20–1000 kX/sq depending on a position of the measured
point. Considering the above values of Rsh for the epilayer,
the low-ohmic part of the substrate largely contributes to the
SNMM measured dependences f(x,y) and Q(x,y) for the edge
area of sample De3. The developed SNMM method yields a
resistance value for the epilayer that is not distorted by the
substrate. According to the data in Fig. 5(b), the epilayer of
sample De3 is, apparently, sufficiently homogeneous, and the
observed spread in values is most likely related to an error in
the SNMM measurements of high-ohmic structures with
Rsh > 100 kX/sq. By estimates, the limit of Rsh measurement
for our SNMM is 500 kX/sq, i.e., the Rsh values obtained
FIG. 5. Scan profiles of the epilayer resistance for samples (a) De2 and (b)
De3. Right-hand insets of (a) and (b) show scanning lines 1–3 and the posi-
tion of crosses I–V under VDP-L measurements. In the right-hand inset of
(a), the dark oval indicates a high-ohmic region. The left-hand inset of (a)
shows a Hall cross structure.
J. Appl. Phys. 121, 164503 (2017)
for De3 are close to the limit. The above estimate of the cut-
off value, obtained from the fluctuating sensitivity threshold
of our SNMM with respect to parameters f and Q, is suitable
for testing a conducting film deposited on any dielectric sub-
strate. At Rsh > 500 kX/sq, parameters f and Q measured for
the film-substrate system do not differ, within a fluctuation
error, from similar parameters for a bare dielectric substrate.
For a bulk homogeneous conducting sample, such as the sub-
strates under study here, a similar estimation of cutoff resis-
tivity yields qc  15 kX cm. At q > qc, the SNMM perceives
the substrate as a dielectric (point Ds0 in Fig. 1(c)). The
limit of measurable characteristics can be increased through
more rigorous temperature/vibration stabilization and other
improvements of SNMM. In particular, modern nanometer-
resolution devices6,7 have a higher sensitivity threshold since
they are designed to measure significantly smaller variations
of the SNMM resonance curve than mid-resolution micro-
scopes. Naturally, these devices are much more expensive
and harder to be operated. The measurement capabilities of
our SNMM proved fairly adequate to serve the purpose of
this work.
The findings for sample De2 give evidence of the fact
that defects in a substrate crystal structure influence the elec-
trical properties of an epilayer. SNMM scanning results in
Fig. 5(a) show the inhomogeneity of epilayer resistance Rsh.
The high-ohmic region of the layer coincides with the area
of structural inhomogeneity on the substrate Ds2 (see inset
in Fig. 4(b)). Note that in this case, the boron concentration
profile NB(z), measured by SIMS in three points on the sam-
ple both in the defect region and beyond, proved to be practi-
cally the same (Fig. 4(b)). So, a substrate crystal structure
defect does not affect the impurity content while reducing
either a concentration or mobility of charge carriers in the
corresponding region of the epilayer. The VDP-S measure-
ment yields resistance Rsh ¼ 8 kX/sq, which characterizes
only the near-edge area of the epitaxial film and is in accord
with the corresponding SNMM data in Fig. 5(a), obtained for
this region.
Rather, low resistance values obtained from the edge
region of the epitaxial film in sample De2, Rsh  7–8 kX/sq,
can be related to a highly doped delta-layer. The fact that
SNMM and VDP-S measurements yielded close Rsh results
for this region means that the VDP-S data can be used for
the estimation of electrophysical parameters in it. Taking the
delta-layer thickness t ¼ 3.5 nm (see SIMS data in Fig. 4(b)),
from the VDP-S data, we found the following characteristics
for the delta-layer: resistivity, q ¼ Rsht  2.5  103 X cm;
hole concentration, Np  1.7  1020 cm3; and mobility,
lH  15 cm2/(V s). With the peak boron concentration being
NB  3  1020 cm3 (see Fig. 4(b)), the dopant ionization
was estimated at 57%. The obtained characteristics do not
contradict the available literature data on the conductivity of
a delta-layer in diamond.37–43 However, an unambiguous
conclusion that these characteristics pertain to the delta-layer
can be made only based on further research, as there may be
other conductivity channels in the epilayers of diamond, for
example, those arising through the addition of electrically
active hydrogen on interfaces.44–46
164503-6 Reznik, Korolyov, and Drozdov
TABLE I. VDP-L measurements of electrical parameters for sample De3
and substrate Ds3.
Number of Rsh, kX/sq lH, cm2/(V s) Ns, 1/cm2
cross (sample/substrate) (sample) (sample)
I 17/17 1180 3.2  1011
II 5/4 680 1.5  1012
III 130/- 18 2.8  1012
IV 330/- … …
V 60/- 31 3.4  1012
Thus, SNMM measurements yielded information on the
epilayer, which is undistorted by the shunting effect and
inhomogeneous conductivity of the substrate. This allowed
us to study the electrophysical properties of the epilayer and
delta-layer with a higher accuracy. We were also able to cor-
rectly use the data from measurements performed by alterna-
tive methods. In particular, comparing the photograph of
substrate Ds2 in Fig. 2(b) with the results of SNMM scan-
ning of sample De2 in Fig. 5(a) has led us to a conclusion
that the high-ohmic region of the epilayer is most likely due
to a substrate defect. On the other hand, relating the VDP-S
measurement data to the low-ohmic near-edge region of
sample De2, based on the SNMM results, allowed us to, a
certain degree of reliability, estimate the electrical parame-
ters of the delta-layer.
The SNMM results are confirmed by the VDP-L meas-
urements. In Table I, we provide the measured values for the
layer resistance Rsh, mobility lH, and sheet density Ns of free
carriers in structure De3 and its substrate Ds3. The position of
crosses I-V is shown in the insets in Figs. 3(b) and 5(b). The
obtained values for structure De3 are determined by the con-
ductivity of both the epilayer and the substrate. To identify the
contributions from either of these two conductivity channels,
we measured the substrate resistance after the epitaxial layer
had been fully removed. It should be noted that VDP-L meas-
urements on structures with a conducting substrate yield
approximate data. The use of the VDP technique requires that
ohmic contacts be formed at the edges of a test structure,
which was not the case in our VDP-L measurements of sam-
ples with a high conductive substrate. The VDP-L studies con-
firmed the inhomogeneity of conductivity in substrate Ds3. Its
high-ohmic region is located in the vicinity of crosses III-V,
where measurements failed due to a high resistance between
the contacts of the cross. The results Rsh ¼ 60–330 kX/sq for
sample De3 with an epilayer, which were obtained for crosses
III-V, are in agreement with the SNMM data (see Fig. 5(b)),
i.e., they refer to the layer. Resistance Rsh ¼ 4–17 kX/sq, as
well as concentration Ns and mobility lH, measured on
crosses I and II, characterizes only the substrate that shunts a
higher resistance of the epilayer. The same conclusion is
made based on the SNMM data given in Figs. 3(b) and 5(b).
Knowing the substrate thickness and the sheet density Ns,
measured using Hall crosses I and II, we can estimate a bulk
concentration of free carriers in the substrate conducting area,
which is N  1013–1014 1/cm3. The VDP-S resistance mea-
surement on sample De3 with an epilayer yields Rsh ¼ 20 kX/
sq, which is conditioned by the low-ohmic edge region of the
J. Appl. Phys. 121, 164503 (2017)
TABLE II. VDP-L measurements of Rsh for sample De2.
Number of cross Rsh, kX/sq
I 54
II 310
III 4500
IV 47
V Cross damaged
substrate. So, we see that non-local VDP studies of an epilayer
in substrates with inhomogeneous conductivity may not be
informative enough. SNMM measurements in the same condi-
tions yield objective information on a layer resistance.
The results of the VDP-L resistance measurements on
sample De2 are presented in Table II. The position of Hall
crosses I-V is shown in the inset in Fig. 5(a). The conclu-
sions made from the SNMM studies were also found to be
true for sample De2: the maximum resistance is observed at
crosses II and III over the defect region of the substrate; out-
side this region (crosses I and IV), the epitaxial layer resis-
tance decreases. The obtained SNMM and VDP-L values
of Rsh show a mutually satisfactory agreement (compare Fig.
5(a) with the data in Table II). The only exception is point
III at which the difference in the measurement result by an
order of magnitude is apparently connected with an error in
the SNMM and VDP-L techniques when measuring high val-
ues of resistance Rsh.
CONCLUSION
In this paper, it has been demonstrated that the devel-
oped SNMM technique is an effective tool for quantitative
characterization of semiconductor doped structures. The
major advantages of our mid-resolution SNMM include local
and nondestructive non-contact diagnostics that show up
most vividly in the process of developing the technologies
for the fabrication of new materials. One example of such a
material is semiconductor diamond. We have studied boron
delta-doped CVD diamond structures epitaxially grown on
an HPHT substrate. Working out a technology for doping
and characterization of diamond structures involves great
difficulties related, in particular, to small sizes, macroscopic
defects, and laterally inhomogeneous conductivity of sub-
strates. Thus, the VDP-S method proved to be least informa-
tive in the case when the substrate shunted the doped
epilayer due to high conductivity in the edge region. VDP-L
measurements allowed us to obtain local data only at some
points in the central part of a sample surface, provided that
the epilayer on the rest of the substrate surface had to be
removed. The SIMS technique yielded high homogeneity of
the doping impurity concentration when the conducting
properties of a structure were strongly inhomogeneous. In
these conditions, when the characterization of diamond sam-
ples proved to be rather complicated, the SNMM merits
showed up most vividly. Our SNMM method enabled the
mapping of resistance Rsh of a delta-doped epilayer of dia-
mond grown on a defective substrate with an inhomogeneous
conductivity.
164503-7 Reznik, Korolyov, and Drozdov
One of the primary claims of this work is that the
SNMM method enables spatially resolved characterization
of the sheet resistance of an epilayer when the supporting
substrate has shunting and inhomogeneous conductivity.
With the method described in Ref. 20 (when only one
unknown parameter of a test structure is to be determined),
such testing was possible only by independent scanning of a
bare substrate and a substrate with the grown epilayer.
However, the SNMM technique has potential for solving
more complicated inverse problems of testing structures with
a few parameters being measured simultaneously. The diag-
nostics of multiparametric objects involves complex meas-
urements, for example, over some frequency ranges or using
a number of probes differing in the aperture size. A possibil-
ity of solving such problems with SNMM was demonstrated
in Ref. 47 through computer modeling.
ACKNOWLEDGMENTS
The authors are grateful to colleagues from the laboratory
of Professor A. L. Vikharev (Institute of Applied Physics RAS,
N. Novgorod, Russia) for fabricating the diamond structures
and to Professor V. I. Shashkin (Institute for Physics of
Microstructures RAS, N. Novgorod, Russia) for organization
and technology provision of VDP-L measurements. We also
thank the above-mentioned colleagues and Professor D. E.
Butler (Institute of Applied Physics RAS, N. Novgorod,
Russia) for useful discussions. This work was supported by
RFBR under Grant No. 15-02-04081 and by the Program of
the Department of Physical Sciences RAS. This research was
based on the equipment of the Common Research Center
“Physics and technology of micro- and nano-structures” at the
Institute for Physics of Microstructures RAS.
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