Nano periodic structure forma-tion in 4H–SiC crystal using femtosecond laser double-pulses
The photo-induced periodic nano structure inside 4H–SiC have been induced by a femtosecond double pulse train. The alignment of the periodic structure is in the direction independently from crystal orientation. In particular, FE-SEM analysis revealed that the periodic structure on the fractured surf...
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irk-123456789-1671032020-03-16T01:25:41Z Nano periodic structure forma-tion in 4H–SiC crystal using femtosecond laser double-pulses Kim, E. Shimotsuma, Y. Sakakura, M. Miura, K. Получение, структура, свойства The photo-induced periodic nano structure inside 4H–SiC have been induced by a femtosecond double pulse train. The alignment of the periodic structure is in the direction independently from crystal orientation. In particular, FE-SEM analysis revealed that the periodic structure on the fractured surface can be classified into two categories of the polarization-dependent and polarization-independent. Фотоіндукована періодична наноструктура всередині 4H–SiC була індукована фемтосекундним подвійним імпульсом. Вирівнювання періодичної структури відбувалося в напрямку, незалежному від орієнтації кристала. Зокрема, аналіз FE-SEM показав, що періодичну структуру на тріщинуватій поверхні можна розділити на дві категорії: поляризаційно-залежної та незалежної від поляризації. Фотоиндуцированная периодическая наноструктура внутри 4H–SiC была индуцированна фемтосекундным двойным импульсом. Выравнивание периодической структуры происходило в направлении, независимом от ориентации кристалла. В частности, анализ FE-SEM показал, что периодическую структуру на трещиноватой поверхности можно разделить на две категории: поляризационно-зависимой и независимой от поляризации. 2018 Article Nano periodic structure forma-tion in 4H–SiC crystal using femtosecond laser double-pulses / E. Kim, Y. Shimotsuma, M. Sakakura, K. Miura // Сверхтвердые материалы. — 2018. — № 4. — С. 41-50. — Бібліогр.: 35 назв. — англ. 0203-3119 http://dspace.nbuv.gov.ua/handle/123456789/167103 544.137/.537:666.652 en Сверхтвердые материалы Інститут надтвердих матеріалів ім. В.М. Бакуля НАН України |
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Получение, структура, свойства Получение, структура, свойства |
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Получение, структура, свойства Получение, структура, свойства Kim, E. Shimotsuma, Y. Sakakura, M. Miura, K. Nano periodic structure forma-tion in 4H–SiC crystal using femtosecond laser double-pulses Сверхтвердые материалы |
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The photo-induced periodic nano structure inside 4H–SiC have been induced by a femtosecond double pulse train. The alignment of the periodic structure is in the direction independently from crystal orientation. In particular, FE-SEM analysis revealed that the periodic structure on the fractured surface can be classified into two categories of the polarization-dependent and polarization-independent. |
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Kim, E. Shimotsuma, Y. Sakakura, M. Miura, K. |
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Kim, E. Shimotsuma, Y. Sakakura, M. Miura, K. |
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Kim, E. |
| title |
Nano periodic structure forma-tion in 4H–SiC crystal using femtosecond laser double-pulses |
| title_short |
Nano periodic structure forma-tion in 4H–SiC crystal using femtosecond laser double-pulses |
| title_full |
Nano periodic structure forma-tion in 4H–SiC crystal using femtosecond laser double-pulses |
| title_fullStr |
Nano periodic structure forma-tion in 4H–SiC crystal using femtosecond laser double-pulses |
| title_full_unstemmed |
Nano periodic structure forma-tion in 4H–SiC crystal using femtosecond laser double-pulses |
| title_sort |
nano periodic structure forma-tion in 4h–sic crystal using femtosecond laser double-pulses |
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Інститут надтвердих матеріалів ім. В.М. Бакуля НАН України |
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2018 |
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Получение, структура, свойства |
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Nano periodic structure forma-tion in 4H–SiC crystal using femtosecond laser double-pulses / E. Kim, Y. Shimotsuma, M. Sakakura, K. Miura // Сверхтвердые материалы. — 2018. — № 4. — С. 41-50. — Бібліогр.: 35 назв. — англ. |
| series |
Сверхтвердые материалы |
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AT kime nanoperiodicstructureformationin4hsiccrystalusingfemtosecondlaserdoublepulses AT shimotsumay nanoperiodicstructureformationin4hsiccrystalusingfemtosecondlaserdoublepulses AT sakakuram nanoperiodicstructureformationin4hsiccrystalusingfemtosecondlaserdoublepulses AT miurak nanoperiodicstructureformationin4hsiccrystalusingfemtosecondlaserdoublepulses |
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2025-07-14T23:46:57Z |
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2025-07-14T23:46:57Z |
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1837668048714072064 |
| fulltext |
ISSN 0203-3119. Сверхтвердые материалы, 2018, № 4 41
UDC 544.137/.537:666.652
E. Kim1, *, Y. Shimotsuma1, **, M. Sakakura2, K. Miura1
1Department of Material Chemistry, Graduate School of Engineering,
Kyoto University, Kyoto, Japan
2Next Generation Laser Processing Technology Research
Association, Kyoto, Japan
*eunhokim@func.mc.kyoto-u.ac.jp
**yshimo@func.mc.kyoto-u.ac.jp
Nano periodic structure formation in 4H–SiC
crystal using femtosecond laser double-pulses
The photo-induced periodic nano structure inside 4H–SiC have been
induced by a femtosecond double pulse train. The alignment of the periodic structure is
in the direction independently from crystal orientation. In particular, FE-SEM analysis
revealed that the periodic structure on the fractured surface can be classified into two
categories of the polarization-dependent and polarization-independent.
Keywords: 4H–SiC, periodic nano structure, femtosecond laser,
double pulse, phase change, semiconductor.
INTRODUCTION
Among the wide bandgap semiconductors, SiC is very hard mate-
rial and has excellent properties such as high breakdown voltage and ther-
mal/chemical stability. Therefore, it is expected as a key material for next
generation power devices. On the other hand, SiC is also known as a hardly
processed material because of high hardness property. Recently, the conventional
wire-saw slicing technique is employed to fabricate semiconductor wafer from
ingot [1–4]. Such technique also employed for SiC wafer, which has advantages
for mass production from its high throughput [5]. The other approach of smart cut
method using proton also proposed to settle some negative issues for SiC substrate
[6–8]. At the recent time, a stealth dicing method has been used to cut the
fabricated semiconductor device chip on the wafer using an ultrashort pulse laser
[9–11], this dicing technique has also attractive to improve the production for SiC
applications [12, 13]. In recent years, material modification using ultrashort pulse
laser has attracted attention because there is possibility of applying it with potential
photonic application. The structural changes induced by femtosecond laser pulses
have been studied about various transparent bulk materials at wavelength from
visible to NIR ranging from glass [14, 15], diamond [16], TeO2 [17], ZnO [18],
GaN [19], 4H–SiC [20], GaP [21], Si [22]. In the case of SiC, the formation of the
nano voids due to micro-explosion and periodic structure has been reported [20]. It
is known that periodic nano structures can be formed in indirect semiconductors or
dielectric, and their arrangement direction is divided vertical [15, 17] or horizontal
[20–22] with respect to the polarization direction of light. The dominant
mechanism on the dependence of the arrangement direction in the polarization
direction is still not clear. Therefore, we elucidated the mechanism of periodic
structure formation by investigating 4H–SiC more in detail from previous research.
© E. KIM, Y. SHIMOTSUMA, M. SAKAKURA, K. MIURA, 2018
http://stmj.org.ua 42
[20] In this study, we investigated the modified structure in the 4H–SiC using
femtosecond pulse laser with double pulse train technique [23]. We confirmed that
the periodic nano structure is aligned not only depend on the polarization direction
of the light but also in the scanning direction as a circular shape regardless of
single- and double-pulse-trains with strong fluence rather than previous report.
Moreover, the periodic nano structure also aligned in the polarization direction
without depending on the crystal orientation.
EXPERIMENTAL
In the study, we used commercially available nitrogen-doped 4H–SiC (0001)
wafer with a thickness of 420 μm (Tankeblue semiconductor). We prepared two
types of samples, a 5×5 mm square chip cut from wafer for c-plane (0001), and a
0.4×5 mm rectangular rod using c-plane chip in which vertically set up then pol-
ished it by CMP method for a-plane (11 2 0). The detail procedure of laser-slicing
method was described our previous report. [23] The experiments were carried out
using femtosecond laser oscillator equipped with a regenerative amplifier (Cyber-
laser; IFRIT) The center wavelength, pulse duration (τpulse) and pulse repetition rate
of this laser system were 780 nm, 220 fs and 1 kHz, respectively. The schematic
illustration of 4H–SiC crystal structure and irradiation direction is shown in Fig. 1.
c�axis
a�axis
a
c�plane {0001}
a�plane {1120}
m�plane {1100}
k
w
k
w
b
Fig. 1. Crystal structure of 4H–SiC (a), main crystal planes of c- , m-, a-plane (b).
To investigate the optimal condition for (11 2 0), the τpulse was changed from 220 fs
to 1 ps. Moreover, to enhance the light-matter interaction, we configured the Mach-
ISSN 0203-3119. Сверхтвердые материалы, 2018, № 4 43
Zehnder type of double pulse optical setup [24]. The time delay (τdelay) between
femtosecond double pulses was controlled by using an optical delay line. The total
pulse energy (Epulse) of the equally divided double pulses was tuned by neutral
density filter. To compensate the spherical aberration due to the high refractive
index of SiC (n0 = 2.6 at λ = 780–800 nm), we used a spatial light modulator
(LCOS-SLM, Hamamatsu Photonics; X10468). The pre-calculated CGH for the
correction of spherical aberration at the focal depth of 260 μm was displayed on
LCOS-SLM. The laser beam was focused inside a SiC wafer with a 50× objective
(Nikon, LU Plan Fluor; NA 0.80, Transmittance ≈ 80 % at 800 nm). Since we have
compensated the spherical aberration, the beam diameter obtained to be approxi-
mately 1.2 μm. To reveal the orientation dependence of the periodic structure, the
laser pulse was induced SiC inside sample to the [0001] (c-plane) or [11 2 0] (a-
plane) directions. The typical laser energy before objective lens was to be 10 μJ, a
typical laser fluence was calculated to be 5.7×102 J/cm2. The absorption coefficient
of 4H–SiC at 780 nm was set to be 26 cm−1 for c-plane and 47 cm–1 for a-plane,
respectively [25]. The laser-written tracks at a spacing of 25 μm in the SiC wafer
were typically formed by scanning the wafer relative to the focus at 100 μm/s with
direction to {11 2 0}. After laser writing, the samples were fractured off in the
plane perpendicular to the laser-written tracks using instant glue on the sample
surfaces and SUS-holding locking jig. The fractured surface morphology was char-
acterized by FE-SEM (JEOL; JSM-6705F). To reveal the detailed structural
changes by the laser writing, the observation by using an aberration corrected high
resolution transmission electron microscope (JEOL; JEM-2200FS) was performed.
RESULTS AND DISCUSSIONS
Threshold for (11 2 0) SiC Crystal Internal Laser-Processing
In order to optimize the laser-processing condition for a-plane, we investigated
the damage threshold by using single- or double-pulse trains with different Epulse.
The polarization of electric field is set to parallel to the c-axis. In the case of single
pulse train, we were unable to modifying or impossible to processing the a-plane
inside even if the pulse duration increasing until 1 ps. It might be higher threshold
than that of the c-plane. This phenomenon is similar with GaN single crystal [19],
which was also several times higher than c-plane irradiation. In the case of τpulse =
220 fs using double-pulse-trains, we were unable to apply the structural
modification at the focal point even if the Epulse is increasing until the surface has
damaged (Epulse ≈ 22 μJ). We changed the τpulse to enhance the light-matter
interaction in longer time. The processing probability was in steady-state with τpulse
at 1 ps as shown in Fig. 2, a. Figure 2, b shows the process window of Epulse with-
out surface damage from 1 to 20 μJ as a function of τpulse at 1 ps. Exceeding the
20 μJ would be surface damaged. The modified shape was like the inverse triangle.
Both the modified width and height size were increased with increasing the Epulse as
shown in Fig. 2, b. We selected as a optimal condition for a-plane irradiation at
τpulse = 1 ps, τdelay = 3 ps and total Epulse = 10 μJ, respectively. To investigate further
topology of modified structure at the focal point, we did whole area processing
using optimal condition. Then the a-plane sample was exfoliated to normal direc-
tion from focal point.
Cross-Sectional Analysis for Periodic Structure
Figure 3 shows the AFM topology and tilted FE–SEM analysis results of the
structural modification in the propagation to the [0001] direction sample after dry-
http://stmj.org.ua 44
0 5 10 15 20 25
0
20
40
60
80
100
P
ro
ba
bi
lit
y,
%
Total pulse energy, μJ
1
2
3
a
0 5 10 15 20 25
0
20
40
60
80
100
120
M
od
if
ie
d
sc
al
e,
μ
m
Total pulse energy, μJ
1
2
b
Fig. 2. The probability of internal processing rate of (110) 4H–SiC as a function of the total pulse
energy (a); the τdelay set to minimum without overlap the each pulse to maximizing the light-
matter efficiency; 500 fs/2 ps (1), 750 fs/2 ps (2), 1 ps/2 ps (3). The size of width (1) and height
width (2) of the internal processing as a function of total pulse energy (b); the gray area since
22 μJ indicates surface damaged; the τdelay between picosecond double pulse (τpulse = 1 ps) was
set to 3 ps.
E kw
a b c
Fig. 3. Cross-sectional view of structural modifications in 4H–SiC (0001) plane after dry-etched
using O2/SF6 for 30 s. AFM topology analysis (a), tilted FE-SEM image (b) and magnified image
(c) from white-box in (b). The laser writing conditions by the double-pulse trains: Epulse = (5 +
5) μJ, τpulse = 220 fs, τdelay = 2 ps.
etched with double pulse train. The modified area was selectively etched about
100 nm. The cracks to the cleaver plane direction and nano voids of several tens
nano-meter diameter were observed by O2/SF6 dry etching process for 30 s. It was
convincing to think that considering the presence of amorphous Si and C previ-
ously confirmed by Raman analysis [23, 26], which was able to etch easily by SiC
amorphization. Since the difference in density of dangling bond and reactivity on
the surface causes a difference in etch rates between crystal and amorphous SiC
[27]. Moreover, we confirmed that nano voids were formed in the modified region
regardless of the pulse trains. In order to investigate the periodic nano structure,
HRTEM analysis was performed with the sample vertically cut by focused-ion-
beam. Figs. 4, a–c set and Figs. 4, d–f set are shows cross-sectional HRTEM with
FFT analysis of the samples induced by single- and double pulse trains, respec-
tively. There appears to be considerable difference of modified phase between
single- and double-pulse-trains irradiation. In case of single pulse train, the FFT
analysis on the area “b” (dark-contrast in Fig. 4, a) clearly shows as 4H–SiC crys-
tal form (see Fig. 4, b). On the other hands, the other bright-contrast on the area “c”
ISSN 0203-3119. Сверхтвердые материалы, 2018, № 4 45
shows as amorphous ring pattern. (see Fig. 4, c). We calculated the lattice spacing
d from FFT analysis that the lattice spacing of (0004) c/4 (~ 0.244 nm) slightly
compressed than that of non-stressed (~ 0.251 nm) lattice. In case of double pulse
trains, the modified area was changed into poly-crystal. Figure 4, e FFT image
shows diffraction pattern on the modified area of double pulse train sample that.
There are two angle of (2 2 00) and (2 2 00)* spots we found in the “region e”. In
particular, the spot reveal not only rotated c/4 and a/2 but also some alternative
phases (d = 0.227, 0.316, 0.363, 0.498, 0.638 nm). We also found the elongated
spot in the high contrast area (see inset of Fig. 4, f). The FWHM of diffraction spot
intensity increased by 3 times from 0.30 to 0.98 nm–1 at the time of non-irradiation.
We suppose such extended spots parallel to the axial direction caused by presence
of axial defects. [28] According to literature, the lattice spacing for d = 0.316 and
0.638 nm are supposed to be graphite (0002) and (0001), respectively. We com-
pared the lattice spacing d = 0.363 nm from previous report that the lattice constant
is very similar with nano-crystal diamond (d ≈ 0.358 nm) [29]. Based on the local
heating and local high-pressure environment by ultrafast pulse laser, the nano dia-
mond might be possible to create in the irradiated center. Furthermore, we also
found the d = 0.498 nm forbidden Bragg scattering spot of (0002) 4H–SiC. We
assumed that both (0001) graphite and (0002) 4H–SiC are apparently due to the
double Bragg reflection occurring inside the disordered crystal [30]. The lattice
spacing d = 0.227 nm is still unidentified structure phase. We also measured TEM-
EDS analysis to investigate the element distribution change of silicon and carbon
in the modified area. There are no significant change found the carbon distribution
in both single- and double-pulse-train samples. On the other hand, although there
were no significant change found the silicon distribution in the modified area, only
silicon decreased in nano void.
E
kw
a b c
E
kw
d e f
Fig. 4. Cross-sectional HRTEM images of the laser-written scanning induced by single- (a) and
double-pulse-trains (d). FFT images of (b) and (c) are corresponding with region b and c in (a),
respectively. The FFT result of (e) and (f) are corresponding with region e and f in (d). The laser
writing conditions by the single-pulse trains: λ = 780 nm, Epulse = 10 μJ, τpulse = 1 ps. The laser
writing conditions by the double-pulse trains: Epulse = (5 + 5) μJ, τpulse = 220 fs, τdelay = 2 ps.
http://stmj.org.ua 46
FE-SEM Analysis on the Exfoliated Surface
To investigate the modified structure in the wide area, we have also carried out
the FE-SEM analysis on the vertically fractured sample surface. Figure 5, a shows
SEM of the upper side surface of fractured sample induced by double-pulse-train
irradiation. We can see there are periodic nano structure with beyond the
diffraction limit. The periodic structure on the region A aligned in the direction
parallel to the laser polarization direction. In addition, we also found polarization-
independent structure; the shape is circular with direction to the laser-scan on the
region B (see also Fig. 5, b). We suppose the modified region classified as two
types of periodic structure; a curve type oriented in the scanning direction and a
linear type oriented in the laser polarization direction. A similar phenomenon has
reported in fused silica glass. Mcmillen et al. reported photo-induced periodic
structures inside fused silica aligned with a circular or pseudo-random shape by
azimuthal or radial polarization [31]. This is the first revealed phenomenon in the
semiconductor instead of glasses. On the other hands, there are also much of large-
scale (~ 100 nm) nano void on the fractured surface that diameter was bigger than
cross-section TEM analysis (~ 20 nm) [20] (see Fig. 5, c). We assume that the
difference of diameter is due to the different sample preparation method or
30 times higher (570 J/cm2) fluence than other group (17.7 J/cm2). Note that such
three structures also observed on the fractured surface induced by single-pulse-
train irradiation. We speculated these characteristic distributions can be accounted
as follow. If the laser applied in the focal depth, a periodic structure formed as a
direction parallel to the laser polarization by light-matter interaction at the upper
focal depth (region A). At the same time, some complicated processes such as the
self-focusing due to Kerr effect and self-defocusing by plasma generation, disso-
ciation of Si–C bonding, defect, and local-strain, also can occur during irradiation
when the peak power of laser is above the critical point (Pcr) at the focal depth.
These might be allowing periodic structure forming as polarization-independently
(region B).
E
kw
a
E
kw
kw
E
kw
kw
b
c
Fig. 5. FE-SEM image of exfoliated 4H–SiC surface induced by double-pulse-trains: top-surface
(a), bottom-surface (b–c). Inset shows magnified image of the white box area in (a). The laser
writing conditions by the double-pulse trains: Epulse = (5 + 5) μJ, τpulse = 220 fs, τdelay = 1 ps.
ISSN 0203-3119. Сверхтвердые материалы, 2018, № 4 47
Based on the inhomogeneous nano plasma model [32, 33], the period of nanos-
tructures in matter is defined as follow:
Λ = λ/2n,
where λ is the laser wavelength, n is the refractive index of material. We obtained
the interval of periodic structure is 154 nm at the wavelength of 800 nm as shown
in Fig. 6. The interval distributed in the range from 130 to 170 nm, which value
agrees with the calculation. In addition, there are no doubled-interval (~ 300 nm) of
periodic structures found on the fractured sample, which originated by second or-
der wavelength [20]. On the contrary, occasionally a half interval (60–80 nm)
structures was observed in the polarization-independent surface. While the high-
spatial-frequency-LIPSS (HSFL) on the surface phenomenon has well-investigated
[34, 35], such similar structure in the matter is relatively under-investigated. In
order to investigate the alignment dependence of the periodic structure with crystal
orientation, we prepared not only c-plane fractured sample but also a-plane frac-
tured one. Figure 7 shows bottom side of fractured a-plane induced by double
pulse trains irradiation. The alignment of periodic structure also arranged with the
direction parallel to the laser polarization. This indicate that alignment of periodic
structure is independent with crystal orientation. The interval of periodic structure
was about 150 nm as well as c-plane.
E
k
w
E E E E
a b c d e
E E E E E
f g h i j
Fig. 6. FE-SEM images of the periodic nano structure on the exfoliated surface: laser polarization
E = 0 (a), 10º (b), 20º (c), 30º (d), 40º(e), 50º (f), 60º (g), 70º (h), 80º (i), 90º (j). The scale bar
indicates 500 μm. The laser writing conditions by the double-pulse trains: Epulse = (5 + 5) μJ,
τpulse = 220 fs, τdelay = 1 ps.
CONCLUSIONS
We have demonstrated the self-organized structure inside 4H–SiC using
femtosecond pulse laser with double-pulse-train technique. In the case of strong
fluence, the periodic nano structure inside 4H–SiC is classified into two categories
of the polarization-dependent and polarization-independent. In particular, align-
ment of the periodic structure is in the direction independently from crystal orienta-
http://stmj.org.ua 48
tion. It was shown that the some other phases were found in the modified area in-
stead of 4H–SiC poly-crystal or amorphous. Moreover, the transformed structure is
not observed significant change of the elemental distribution.
E
k
w
Fig. 7. FE-SEM image of the periodic nano structure on the bottom-surface exfoliated from
a-plane 4H-SiC. Each figure was captured on the individual place, respectively. The arrow in the
figure indicate scan-direction. The laser writing conditions by the double-pulse trains: Epulse =
(5 + 5) μJ, τpulse = 1 ps, τdelay = 3 ps.
This work was partially supported by JSPS KAKENHI (No. 16K13929), Cross-
Ministerial Strategic Innovation Promotion (SIP) Program.
Фотоіндукована періодична наноструктура всередині 4H–SiC була
індукована фемтосекундним подвійним імпульсом. Вирівнювання періодичної структури
відбувалося в напрямку, незалежному від орієнтації кристала. Зокрема, аналіз FE-SEM
показав, що періодичну структуру на тріщинуватій поверхні можна розділити на дві
категорії: поляризаційно-залежної та незалежної від поляризації.
Ключові слова: 4H–SiC, періодична наноструктура, фемтосекундний
лазер, подвійний імпульс, зміна фази, напівпровідник.
Фотоиндуцированная периодическая наноструктура внутри 4H–SiC
была индуцированна фемтосекундным двойным импульсом. Выравнивание периодической
структуры происходило в направлении, независимом от ориентации кристалла. В част-
ности, анализ FE-SEM показал, что периодическую структуру на трещиноватой поверх-
ности можно разделить на две категории: поляризационно-зависимой и независимой от
поляризации.
Ключевые слова: 4H–SiC, периодическая наноструктура, фемтосе-
кундный лазер, двойной импульс, изменение фазы, полупроводник.
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Received 02.11.17
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