Composition and strain analysis of Si1-xGex

core fiber with Raman spectroscopy

Cite as: AIP Advances 8, 065006 (2018); https://doi.org/10.1063/1.5034408
Submitted: 11 April 2018 . Accepted: 25 May 2018 . Published Online: 06 June 2018

Dongyang Wang, Na Chen, Zhenyi Chen, Ziwen Zhao, Fufei Pang, and Tingyun Wang

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 AIP ADVANCES 8, 065006 (2018)

Composition and strain analysis of Si1-x Gex core

fiber with Raman spectroscopy
Dongyang Wang, Na Chen,a Zhenyi Chen, Ziwen Zhao, Fufei Pang,
and Tingyun Wang
Key Laboratory of Specialty Fiber Optics and Optical Access Networks, Joint International
Research Laboratory of Specialty Fiber Optics and Advanced Communication,
Shanghai Institute for Advanced Communication and Data Science,
Shanghai University, Shanghai 200444, P. R. China
(Received 11 April 2018; accepted 25 May 2018; published online 6 June 2018)

The fabrication and characterization of Si1-x Gex core fiber have attracted much atten-
tion because of its great application potential in new optoelectronic devices. In this
work, by assembling two semi-cylindrical monocrystalline Si and Ge rods into a
silica tube, we present a fabrication method to draw Si1-x Gex core silica clad fiber
with graphite furnace. Raman spectra analysis reveals that in all regions of the core
formed the Si1-x Gex alloy. The optical microscopic photograph shows that in the
core of a diameter of 36 µm distributed the bright and dark regions, where it was
further proved by Raman spectroscopy that the bright regions are Ge-rich areas and
the dark regions are rich in silicon. By recording the Raman spectra of consecutive
regions, it was found that with the increase of Ge content (x<0.5) the peak intensity
of Si-Ge mode obviously increases, similar to the intensity of Ge-Ge mode, while
the peak intensity of Si-Si mode decreases. Then we made a quantitative analysis
of the components and strain by mapping the Raman spectra of the fiber core. The
experimental results show that the Ge content mainly distributes between 0.1 and
0.8, concentrating between 0.2 and 0.3, and the strain distribution on the surface is
obtained at the same time. © 2018 Author(s). All article content, except where oth-
erwise noted, is licensed under a Creative Commons Attribution (CC BY) license
(http://creativecommons.org/licenses/by/4.0/). https://doi.org/10.1063/1.5034408

Si1-x Gex alloy has drawn growing attention in photonics field due to mid-wave transparency,1
higher carrier mobility relative to silicon and good photoelectric properties,2,3 which also make it
the ideal material for all-optical devices. Furthermore, continuous adjustable energy gap and optical
properties can be achieved by adjusting the composition of the Si1-x Gex material.4,5 Attracted by
these good features, many researchers started to research the fabrication of Si1-x Gex core fiber. Since
a silica-clad silicon-core fiber has been successfully fabricated with molten-core method by the
Clemson Univ. in 2008,6 lots of methods have been used to draw semiconductor core fiber, such
as high-pressure micro-fluidic chemical vapor deposition by Southampton Univ. and Pennsylvania
State Univ.,7 powder in tube method by Virginia Tech.,8 laser drawing method by Shanghai Univ.9
Recently, by sol–gel technique the bubble-free silicon core fiber was fabricated in Lille1 Univ.10
People were dedicated to research the unitary semiconductor core fiber at first. Then many successful
cases of fabricating binary semiconductor core fiber were reported.11,12 However, Si1-x Gex core fiber
hadn’t been successfully fabricated for a long time, one of the reasons is that it was very difficult to
control the solidification of Si1-x Gex with different composition in the fiber geometry. Until 2016,
using laser recrystallization method, the Si1-x Gex core fibers with 6% and 25% Ge content with a
core diameter of 130 µm were fabricated by Norwegian Univ.13 They analyzed the composition and
structure of Si1-x Gex and gave an approximate distribution of the Si1-x Gex using energy dispersive
X-ray spectroscopy (EDX) and backscattered electron (BSE) techniques. However, the composition

a
Corresponding author: na.chen@shu.edu.cn

2158-3226/2018/8(6)/065006/6 8, 065006-1 © Author(s) 2018

065006-2 Wang et al. AIP Advances 8, 065006 (2018)

and strain distribution inside the fiber core were not obtained quantitatively. In 2017, we reported the
application of Si1-x Gex core fiber in the field of all-optical in-fiber power detection.14 In this paper, we
presented a fabrication method of Si1-x Gex core silica clad fiber by assembling two semi-cylindrical
monocrystalline Si and Ge rods into a silica tube and drawing the fiber with graphite furnace. Then,
we mainly focused our work on the analyzing method of the continuous variation trend of the Ge
content and strain in order to quantitatively obtain the Ge content and strain distribution in the entire
core region.
Composition and stress have great impact on the properties of the Si1-x Gex . Stress affects on
energy band structure15 and lattice vibration,16 while component affects on lattice constant17 and
electron mobility.2 So it is necessary to research distributions of strain caused by stress and compo-
sition for more extensive applications of Si1-x Gex core fiber. As a tool to characterize these factors,
Raman spectroscopy was usually used to record the peaks of Si-Si, Si-Ge and Ge-Ge modes of
Si1-x Gex . As we know, the composition and strain can lead to the shift of the Raman peak,18 so we
can calculate them by analyzing the Raman spectra. The equations used to describe the variety of
Raman spectra with Ge content on unstressed Si1-x Gex alloys were given by Raman spectroscopy and
XRD analysis.19 Because Ge content and strain are independent of each other, these two variables can
be separated. The equations that reveal the variety of Raman spectrum with strain were also given.20
By these equations, the composition and strain information can be obtained by Raman spectra.
By assembling two semi-cylindrical monocrystalline Si and Ge rods into a silica tube, Si1-x Gex
core fiber was fabricated successfully. The fabrication process was shown in Fig. 1(a). Firstly, a pure
silica tube was prepared, one end of which was collapsed in advance. The high-purity monocrystalline
semi-cylindrical Ge and Si rods with an outer diameter 2.5 mm were put together into the silica tube
prepared. Then the preform was connected to the vacuum pump and fixed on the drawing tower.
The vacuum pump provided a negative atmospheric pressure for reducing the oxygen content in the
preform and preventing the core forming oxides. Last, the temperature in the graphite furnace was
raised to 2200◦ C slowly, meanwhile the speed of sending the preform and the speed of drawing fiber
were monitored and adjusted by the computer to make a uniform diameter Si1-x Gex core fiber.
Figure 1(b) shows the fabricated Si1-x Gex core fiber. The interface of core and cladding is a
perfect circle without micro-cracks or gaps. The diameters of the core and the cladding are 36.1 µm
and 134.4 µm respectively. Because Ge has a higher refractive index relative to Si, we can distinguish
from the optical photograph the bright regions are Ge-rich areas and the dark regions are rich in
silicon.
To validate this result, we used LabRAM HR Evolution (HORIBA Jobin Yvon) spectrometer
equipped with a laser of 633 nm and 1800 lines/mm grating to characterize the Raman spectra of
the fiber core. The spectral resolution is around 0.6 cm-1 . The laser with 2.96 mW optical power
was focused onto the sample surface thanks to Olympus 100× (0.9 NA) objective. For improving
spectrum quality, integration time was set to be 3s and the number of accumulation was 2. These
measurement conditions were used for the all the following experiments.

FIG. 1. (a) Fiber draw and preform preparation. (b) Si1-x Gex core fiber end face photograph (100× objective). The inset figure
denotes the locations of each point A-K.
065006-3 Wang et al. AIP Advances 8, 065006 (2018)

FIG. 2. (a) Raman spectra of continuous Points A-J. (b) Raman spectra at Point A (Si-rich regions), C (interface close to
Si-rich), G (interface close to Ge-rich) and J (Ge-rich regions). (c) Raman spectra of Points A-D show the peaks of Si-Si mode
near 500 cm-1 and 480 cm-1 .

As shown in Fig. 2(a), the Raman spectra of some continuous points from the dark regions
(point A) to the bright regions (point J) were recorded, meanwhile the corresponding recorded points
were marked in Fig. 1(b). The reference Raman peaks of Si-Si, Si-Ge and Ge-Ge modes, which
are 300cm-1 , 400cm-1 and 500cm-1 respectively, were lined out with cyan dotted line in Fig. 2(a)
and (b). Figure 2(a) shows that all the spectra have the peak of Si-Ge mode, which reveals that
Si1-x Gex alloy formed all over the core, and it was also certified by Raman spectra with Si-Ge mode
at other random points in the fiber core. In Fig. 2(b), Raman spectra of some special points were
recorded. Through recording the random points in the core, we found that the Raman spectra of
dark regions were similar with Raman spectrum at point A. Point C is the characteristic spectrum
of the interface of dark and bright regions closed to dark regions, while the point G is the char-
acteristic spectrum closed to bright regions. Then, the characteristic spectrum of brighter region is
point J.
Because the Raman peak intensity reveals substance concentration, we can determine Ge content
by analyzing Raman peak intensity varieties. By analyzing Raman spectrum at point A, we find that
Raman peak intensity of Si-Si mode is strong but Ge-Ge mode is weak, so the Ge content is rare at
point A, while point J has a high Ge content owing to a strong Raman peak intensity of Ge-Ge mode
with weak Raman peak intensity of Si-Si mode. By analyzing these continuous points, we know that
Ge content increases gradually from the dark regions (point A) to the bright regions (point J). We can
make a qualitative judgment that the bright regions are Ge-rich areas and the dark regions are rich in
silicon.
Above the variety of Ge content with intensity can be also explain by the relationships between
the peak intensities of the three modes and Ge content. The peak intensity varies only with the Ge
content. The relative intensity is proportional to (1 − x)2 , 2x(1 − x) and x 2 respectively:21
ISi−Si = Aλ · (1 − x)2 (1)

ISi−Ge = Bλ · 2x(1 − x). (2)

IGe−Ge = Cλ · x 2 . (3)
Where, I Si−Si , I Si−Ge and I Ge−Ge are the intensity of Si-Si, Si-Ge and Ge-Ge modes respectively. Aλ ,
Bλ and C λ are undetermined coefficients.
According to the Eqs. (1)–(3), both intensities of Ge-Ge and Si-Ge modes increase gradually
with the increase of Ge content(x<0.5), while the intensity of the Si-Ge mode is reduced at the
high Ge content(x>0.5) but Ge-Ge mode still increases. The growth trend of Si-Si mode inten-
sity with Ge content is opposite to that of Ge-Ge mode. The conclusions are also consistent with
Fig. 2(a).
However, we can see that two peaks appear near Si-Si mode in Fig. 2(a). From the dark regions
to the bright regions, the intensity of Si-Si mode near 500 cm-1 decreases gradually and near the
480 cm-1 increases then decreases gradually. The growth trend of Si-Si mode near 500 cm-1 accords
with the Eq. (1). The appeared peak near the 480 cm-1 is the result of that the Si-Si vibration mode
was affected by the increased Ge content.20 Fig. 2(c) is an enlarged view of the Raman spectra from
065006-4 Wang et al. AIP Advances 8, 065006 (2018)

point A to D, which shows clearly that the peaks of Si-Si mode at 504 cm-1 or 487 cm-1 only change
in intensity with little peak shift.
After we analyzed the Ge content by the Raman peak intensity of the various points, we quanti-
tatively analyzed composition and strain by the shifts of Raman peak position all over the core. Many
researchers have interpreted the relationship between composition, strain and Raman spectra. In these
researches, people found that each spectrum of Si1-x Gex has more or less deviation relative to the
standard spectrum. Differences in material component and inner stress, which are considered as the
main reason, will cause change in the lattice constant, resulting in change of Raman spectrum. Based
on the existing Raman spectra analysis of Si1-x Gex in the literature,22 the Ge content and the strain
can be calculated by the Raman spectrum. A set of binary linear equations with six undetermined
coefficients were given.20
ωSi−Si = ω0Si−Si − A1 x + b1 ε// (4)

ωSi−Ge = ω0,x→0
Si−Ge
− A2 x + b2 ε// (5)

ωGe−Ge = ω0Ge−Ge − A3 x + b3 ε// (6)

Where x is the Ge content and ε // is the in-plane strain. A1 , A2 and A3 are the undetermined coefficients
linking the shift of the Si–Si, Si–Ge and Ge–Ge modes with Ge content, while b1 , b2 and b3 are the
Raman peak position shift with strain. ωX −Y (where X, Y stand for Si and Ge) is the Raman peak
position, while ω0X−Y is the reference peaks of Si-Si and Ge-Ge modes and ω0,x→0 Si−Ge
is the reference peak
position of Si-Ge mode for x close to 0. ω0 = 520cm , ω0,x→0 = 400cm ω0Ge−Ge = 282.5cm−1
Si−Si −1 Si−Ge −1

has been given in some papers.22,23

In the equations above, the reference range of coefficients has been given.23,24 Due to the differ-
ences in experimental conditions of different researches, it is necessary to find a set of coefficients
corresponding to the specific experimental data. According to Eqs. (4) and (6), x and ε // can be
calculated.    
− ωSi−Si − ω0Si−Si b3 + ωGe−Ge − ω0Ge−Ge b1
x= (7)
A3 b1 − A1 b3
   
ωSi−Si − ω0Si−Si A3 + ωGe−Ge − ω0Ge−Ge A1
ε// = (8)
A3 b1 − A1 b3
The x and ε // of Eq. (5) were substituted by Eqs. (7) and (8).
A2 b3 − A3 b2 Si−Si A1 b2 − A2 b1 Ge−Ge
ωcal
Si−Ge
= ω0,x→0
Si−Ge
− ω − ω
A3 b1 − A1 b3 A3 b1 − A1 b3
(A2 b3 − A3 b2 )ω0Si−Si + (A1 b2 − A2 b1 )ω0Ge−Ge
+ (9)
A3 b1 − A1 b3
For each set of coefficients, ωSi−Si , ωGe−Ge of the Eq. (9) were substituted by the data of Raman
spectrum, then ωcal
Si−Ge
was calculated. Compared with ωSi−Ge , the coefficients were valid if they differ
-1
by 0.6cm (taking into the spectral resolution and the calculation error). In addition, another sets
of Raman spectra data were randomly selected for further calculations. If the set of coefficients
is suitable for more than 97% of the spectra selected, it was considered that the set of coeffi-
cients was reliable. After the calculation, the equations with determined coefficients were given as
below.
ωSi−Si = 520 − 62x − 885ε// (10)

ωSi−Ge = 400 + 25x − 546ε// (11)

ωGe−Ge = 282.5 + 27x − 413ε// (12)

Then, we mapped the Raman spectra of 80×80 points in the core of 40 µm×40 µm. As shown in
Fig. 3, the coordinate axis of (a)-(h) represents the geometrical dimension of the core, whose unit is
µm. Each pixel grid in the diagram represents each spectrum measurement point. The peak intensity
065006-5 Wang et al. AIP Advances 8, 065006 (2018)

FIG. 3. (a)-(c) The peak intensity distributions of Ge-Ge, Si-Ge and Si-Si modes respectively. (d)-(f) The peak position
distributions of Ge-Ge, Si-Ge and Si-Si modes respectively. (g) The distribution of calculated Ge content. (h) The distribution
of calculated strain. (i) The column chart of Ge content.

and position information of each point were separated into the following figures. Figure 3(a)–(c)
are the peak intensity distribution of Ge-Ge, Si-Ge, Si-Si modes, while (d)-(f) are the peak position
distributions of Ge-Ge, Si-Ge, Si-Si modes. Through observing the peak intensity distributions of Ge-
Ge, Si-Ge, Si-Si modes in Fig. 3(a)–(c), distributions of Si and Ge inside the core can be confirmed.
Comparing Fig. 3(a) and (c), the regions of stronger intensity of Ge-Ge peak are the regions of weaker
intensity of Si-Si peak, while the intensity of the Si-Ge peak is positively related to Ge-Ge at the low
Ge content. This agrees with the previous analysis by the Eqs. (1) and (3).
The Ge content and strain were calculated based on the Eqs. (10), (11) and (12), and the Raman
peak positions of Ge-Ge mode, Si-Ge mode and Si-Si modes. The results are shown in Fig. 3(g)
and (h) respectively. Comparing Fig. 3(g), (a) and (c), the distribution of Ge content obtained by
peak intensities agrees with the calculation result by peak position, which is also consistent with the
observation under microscopy. In Fig. 3(g), we observe that high Ge content agglomerated at the edge
of the core and most of these regions with high Ge content have a stronger positive strain. Positive
strain means tensile stress,25 so these regions present tensile stress. In order to observe clearly the
distribution of Ge content, we have performed statistics on the distribution of Ge content in Fig. 3(i).
In total, 4049 points in the core were counted. The number over the rectangle represents the counts
in this interval. It can be seen from the chart that Ge concentrations are concentrated between 0.2
and 0.3. In the process of fabricating fiber, the same volume Si and Ge were put into the preform,
thus the content of Ge is x = 0.466. However, the value was different from the calculated result,
because Si and Ge didn’t keep the fixed ratio in each cross-section when they were mixed in the silica
tube.
In summary, by assembling semi-cylindrical Si and Ge rods method, Si1-x Gex core silica clad fiber
was directly drawn with graphite furnace. We found that Si1-x Gex alloy formed in the whole regions of
fiber core. In continuous regions, we observed the continuous changes of Raman spectra. By mapping
the Raman spectra of the core, we gave the method to quantitatively calculate the distributions of Ge
content and strain inside the fiber, which will contribute to understand the characteristics of such new
065006-6 Wang et al. AIP Advances 8, 065006 (2018)

material fibers that is of significance in the potential applications of new optoelectronic materials and
devices.
This work is funded by Natural Science Foundation of China (61575120, 61227012, 61475095,
61635006). The authors would like to thank the support of the Key Laboratory of Specialty Fiber
Optics and Optical Access Networks (SKLSFO2017-02).
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